CN106645231A - Light path continuously adjustable catalyst dynamic structure in-suit representation device, and applications thereof - Google Patents
Light path continuously adjustable catalyst dynamic structure in-suit representation device, and applications thereof Download PDFInfo
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- CN106645231A CN106645231A CN201611224614.3A CN201611224614A CN106645231A CN 106645231 A CN106645231 A CN 106645231A CN 201611224614 A CN201611224614 A CN 201611224614A CN 106645231 A CN106645231 A CN 106645231A
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- window
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- continuously adjustable
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- 239000003054 catalyst Substances 0.000 title claims abstract description 86
- 239000000463 material Substances 0.000 claims description 33
- 229910052790 beryllium Inorganic materials 0.000 claims description 17
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 17
- 229920001721 polyimide Polymers 0.000 claims description 17
- 239000004642 Polyimide Substances 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 238000012512 characterization method Methods 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 150000004767 nitrides Chemical class 0.000 claims description 6
- 230000005469 synchrotron radiation Effects 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000009738 saturating Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 238000000833 X-ray absorption fine structure spectroscopy Methods 0.000 claims 3
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000011895 specific detection Methods 0.000 claims 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 abstract 17
- 238000000034 method Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 15
- 238000011065 in-situ storage Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000000235 small-angle X-ray scattering Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000001994 activation Methods 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 238000004998 X ray absorption near edge structure spectroscopy Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910004339 Ti-Si Inorganic materials 0.000 description 1
- 229910010978 Ti—Si Inorganic materials 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 230000003447 ipsilateral effect Effects 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
Landscapes
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a light path continuously adjustable catalyst dynamic structure in-suit representation device. According to the light path continuously adjustable catalyst dynamic structure in-suit representation device, the upper side of a front cover (11) is provided with a long groove type horn mouth; a fixed window flake (1) is arranged on the upper end surface of a fixed window flake pedestal (4); a movable window flake (3) is embedded in the upper end surface of a movable window flake pedestal (7); the movable window flake pedestal (7) is provided with a through hole in the axial direction; the movable window flake pedestal (7) is immobilized in the fixed window flake pedestal (4); a sample cabin (2) is formed among the fixed window flake (1), the fixed window flake pedestal (4), and the movable window flake (3); the fixed window flake pedestal (4) is provided with two axial circular holes, and is communicated with the sample cabin (2); an inlet pipe (5) and an outlet pipe (10) are inserted into the two axial circular holes respectively; a flat backing ring (6) is arranged between a back pressing ring (8) and the movable window flake pedestal (7); the back pressing ring (8) and a back pressing pedestal (9) are connected via screw threads; a back cover (9) and the front cover (11) are firmly connected via bolts. The light path continuously adjustable catalyst dynamic structure in-suit representation device is capable of realizing catalyst dynamic structure in-suit one-line representation, accurate is high, and application range is wide.
Description
Technical field
The invention belongs to a kind of catalyst characterization device and application, and in particular to a kind of continuously adjustable catalyst of light path is moved
State structure in-situ characterization device and application.
Background technology
Most chemical reaction processes belong to catalytic process, and the surface microstructure of used catalyst is to determine its reaction
The vital factor of performance.X-ray occupies highly important status in terms of catalyst structure analysis and characterization.Due to catalysis instead
Process is answered typically to carry out under certain temperature and pressure, but in view of the restriction of previous technical conditions, to actual response condition
It is difficult that lower catalyst active center and its transition rule carry out research.With high brightness, high collimation, the adjustable synchronization of energy
The appearance and development of radiation X-ray, the research to carry out under many normal conditions provides possibility.Synchrotron radiation X light has
The incomparable premium properties of conventional lighting sources, its technological means for differing from one another never can provide catalyst sample by ipsilateral
Microstructure information.Using XANES (X-ray Absorption Near Edge Structure, X-ray absorption near side (ns) knot
Structure) spectrum can be with the chemical state of element in detection sample.And by catalyst EXAFS (Extended X-ray Absorption
Fine Structure, Extended X-ray Absorption Fine Structure) compose and study the original that can obtain absorption Local atomic structure in sample
The information such as subcategory, ligancy and co-ordination distance, this can be not only used for studying preformed catalyst crystalline state and amorphous knot
Structure, can be also used for the crystallite or impalpable structure of Study of Catalyst.The high collimation of synchrotron radiation X-ray, the adjustable advantage of energy,
Even more routine XRD (X-ray Diffraction, X-ray diffraction) is incomparable；Height collimation ensure that high explanation, and energy is adjustable
To carry out anomalous scattering；This be all structure elucidation more accurately and reliably.High-resolution XRD can provide catalyst crystal structure ginseng
The information such as number, phase transition process, grain size, crystal grain orientation and micro-structural (point defect, dislocation, planar defect).SAXS/WAXS
(Small and Wide Angle X-ray Scattering, low-angle scattering of X-rays and wide-angle are scattered) can be used to investigate catalysis
The growth course of presoma nanoparticle structure, the evolution of property and photocatalyst crystals in agent crystallization process.By using these
Technology, microstructure and its change of the Study of Catalyst in processes such as roasting, activation, reaction and regeneration, contributes to our and differentiates
Its catalytic active center, understands its development law.Research and development of these information to new catalyst and catalytic reaction process
It is indispensable.
The sample cell that patent ZL200910075167.3 is related to, does not have medium access way, it is impossible to carry out to have gas or
The catalytic reaction that liquid medium is participated in carries out in-situ characterization；When it is used for XRD signs, the information of wide-angle cannot be obtained.Patent
The sample cell of ZL200910075168.8, when carrying out being related to the experiment of high-pressure gas medium, the dead volume on X-ray road is larger,
Have a strong impact on signal to noise ratio so that the quality of data is reduced when in-situ characterization is tested, it is difficult to play the huge advantage of synchrotron radiation X light.
The content of the invention
It is an object of the invention to provide a kind of catalyst dynamic structure online sign in situ, degree of accuracy height, scope of application width
The continuously adjustable catalyst dynamic structure of light path online characterization apparatus in situ and application
The device and method of this is in room temperature～500 DEG C, under the conditions of normal pressure～6MPa, in online mode in situ to system
Crystallization process during standby catalyst, metal oxide catalyst roasting process, the activation of various catalyst, reaction, regeneration were waited
Journey XAFS (X-ray absorption fine structure), XRD (X-ray diffraction), SAXS (low-angle scattering of X-rays), (X is penetrated SAXS/WAXS
Low angle scattering of x ray x and wide-angle diffraction) studied.Monitoring catalyst structure (particularly surface microstructure) during these
Change.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path of the present invention, it includes determining window, sample
Storehouse, moves window, determines window seat, and inlet pipe, plain cushion ring moves window seat, rear pressure ring, bonnet, outlet pipe, protecgulum, it is characterised in that protecgulum
There is longitudinal horn mouth upside, under it is little big, determine window positioned at window seat upper surface is determined, dynamic window is embedded in dynamic window seat upper end
Face, dynamic window seat axially has through hole, and dynamic window seat is located to be determined in window seat, and is threaded connection, determine window, determine window seat and
Form sample bin between dynamic window, determining window seat has symmetrical 2 axial circular holes, and communicates with sample bin, inlet pipe, outlet pipe respectively with
2 axial circular holes are communicated, and rear pressure ring is located at dynamic window seat lower end, there is plain cushion ring between rear pressure ring and dynamic window seat, rear pressure ring with
Afterwards wedge is connected with fastening with thread connection, bonnet and protecgulum.
Bonnet as above is uniformly distributed 4-8 large through-hole with protecgulum, and bolt is connected bonnet and protecgulum by large through-hole
Connect fastening.In bonnet and protecgulum 2-6 small through hole is uniformly distributed for placing cartridge heater.
Determine window and determine between window seat as mentioned above, between plain cushion ring and dynamic window seat, between plain cushion ring and rear pressure ring
There is sealing gasket, its material can be polytetrafluoroethylene (PTFE), polyimides, soft graphite etc., to adapt to the need of different temperatures, pressure
Will.Gasket material is selected according to experimental temperature, and≤250 DEG C can select polytetrafluoro, polyimides, soft graphite；250 DEG C of ＞
And≤400 DEG C select polyimides, soft graphite.
As mentioned above dynamic window seat axially extending bore is interior hexagon, and outer round surface has fine thread, revolved with inner hexagon spanner
During dynamic dynamic window seat, it along determining being threaded into, screwing out for window seat, and then can change the size of sample bin axial direction.Sample
The preferred adjusting range of the size (i.e. X-ray journey) of product storehouse axial direction is：0.01～3mm.
Inlet pipe, outlet pipe tail end are installed through type two and are led to.The logical pipeline that can connect for fluid turnover of through type two, it is also possible to
With dead stifled sealing, it is respectively used to need or there need not be fluid (gas or liquid) medium to be back to back the situation of sample bin.
Afterwards there is interior hexagonal endoporus the lower surface of pressure ring, with during pressure ring, it can be after determining after inner hexagon spanner turn
Wedge is threaded into, screws out.
Determine window, dynamic window and be made up of the metallic beryllium of saturating X-ray material, boron nitride ceramics, polyimides.It is preferential to select gold
Category beryllium, in order to improve the compatibility of window and medium, can be in its surface vapor cvd nitride boron, aluminum oxide, polyimide film.Material
Material is selected according to experiment atmosphere, and metallic beryllium is applied to reducing atmosphere, polyimides, boron nitride ceramics or inner surface cvd nitride
The metallic beryllium of boron membrane is applied to the various atmosphere such as reproducibility, oxidisability, inertia.
Sample bin is used to hold sample.The sample of sample bin can be liquid (colloid, solution, microemulsion etc.), solid-state (
Granular, overall sheet) etc..
The application of the present invention is as follows：
The continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is in room temperature～500 DEG C, normal pressure～6MPa conditions
Lower work, when XRD and XAFS transmission modes are characterized, X-ray is entered from the central axial direction of bonnet, and carries sample message, in the past
The longitudinal horn mouth of lid reaches detector.When XAFS fluorescence modes are characterized, longitudinal horn mouth and sample cell of the X-ray from protecgulum
Determine window to enter into 45 degree of angles, fluorescence signal reaches detector also by the longitudinal horn mouth of protecgulum.
The detailed applying step of the present invention is as follows：
(1), according to the gasket material that choice of experimental conditions is suitable, the material of window and dynamic window, gasket material are determined
Selected according to experimental temperature ,≤250 DEG C are selected polytetrafluoro, polyimides, soft graphite；250 DEG C of ＞ and≤400 DEG C select polyamides
Imines, soft graphite；The material for determining window and dynamic window is selected according to experiment atmosphere, and metallic beryllium is applied to reducing atmosphere, gathers
The metallic beryllium of acid imide, boron nitride ceramics or inner surface cvd nitride boron membrane is applied to reproducibility, oxidisability or inert atmosphere；
(2), in the range of 0.01～3mm, the dynamic window seat of rotation adjusts the size of sample bin axial direction to suitable chi
It is very little；
(3), first by solid-state testing sample loading sample bin, refill and prepare the continuously adjustable catalyst dynamic structure original of light path
Position characterization apparatus；Or the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is first assembled, then liquid sample is injected
Sample bin；
(4) heater element and temperature control galvanic couple, are placed；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6), connecting fluid inlet pipe, outlet pipe, by the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device connection of light path
To in experimental provision；
(7) the actual response condition, in room temperature～500 DEG C, between normal pressure～6MPa, according to required for being characterized catalyst
Design temperature and pressure；
(8) when, using XRD modelings, X-ray is entered from the central axial direction of bonnet, and carries sample message, from protecgulum
Longitudinal horn mouth reach detector；When being characterized using XAFS fluorescence modes, X-ray from the longitudinal horn mouth of protecgulum with determine window
Piece is entered into 45 degree of angles, and fluorescence signal reaches detector also by the longitudinal horn mouth of protecgulum；
X-ray signal that the X-ray signal of detector acquisition of transmission that (9), persistently provided with Synchrotron Radiation, diffraction go out,
The X-ray signal for scattering, you can obtain catalyst in experimentation, the change information of its structure dynamics.
The invention has the advantages that：
(1). using the synchrotron radiation X light of high brightness, realize catalyst dynamic structure online sign in situ.
(2). scope of application width.The catalyst sample of the forms such as solid-state, liquid can be studied；Preparation can be urged
The processes such as crystallization process during agent, metal oxide catalyst roasting process, activation, reaction, the regeneration of various catalyst are entered
Row research.
(3). light path continuously adjustabe, adjustment is easy.Sample to variable concentrations, it is convenient to adjust light path size, to obtain
Optimal signal to noise ratio.
Description of the drawings
Fig. 1 is apparatus of the present invention structural representation.
Fig. 2 is apparatus of the present invention structure schematic top plan view.
As illustrated, 1 is to determine window, 2 is sample bin, and 3 are window, and 4 is to determine window seat, and 5 is inlet pipe, and 6 is plain cushion ring,
7 are window seat, and 8 is rear pressure ring, and 9 is bonnet, and 10 is outlet pipe, and 11 is protecgulum.
Specific embodiment
Embodiment 1：
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path, it includes determining window 1, sample bin 2,
Dynamic window 3, determines window seat 4, inlet pipe 5, plain cushion ring 6, moves window seat 7, rear pressure ring 8, bonnet 9, outlet pipe 10, protecgulum 11, its feature
Be that the upside of protecgulum 11 has longitudinal horn mouth, under it is little big, determine window 1 and be located to determine the upper surface of window seat 4, move window 3 and inlay
In the dynamic upper surface of window seat 7, dynamic window seat 7 axially has through hole, and dynamic window seat 7 is located to be determined in window seat 4, and is connected by screw thread
Connect, determine window 1, determine between window seat 4 and dynamic window 3 formed sample bin 2, determine window seat 4 have it is symmetrical 2 axial direction circular holes, and with
Sample bin 2 is communicated, and inlet pipe 5, outlet pipe 10 are communicated respectively with 2 axial circular holes, and rear pressure ring 8 is located at the dynamic lower end of window seat 7, rear pressure ring
There is plain cushion ring 6 between 8 and dynamic window seat 7, rear pressure ring 8 is connected with rear wedge 9 with thread connection, bonnet 9 and protecgulum 11
Fastening.Concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is polytetrafluoroethylene (PTFE).The material for determining window 1 and dynamic window 3 is metallic beryllium, its surface vapor deposition oxygen
Change aluminium.
(2) dynamic window seat 7, is rotated, the axial direction size of sample bin 2 is adjusted, light path is 3mm on ShiXGuang roads.
(3) the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path, is assembled, bonnet 9 is uniform with protecgulum 12
4 large through-holes of distribution, bonnet 9 and protecgulum 11 are connected fastening by bolt by large through-hole, by colloidal titanium-silicon molecular sieve catalyst
Injection sample bin 2, inlet pipe 5, the tail end of outlet pipe 10 are installed through type two and are led to, the general dead stifled sealing of through type two；
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 4 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6) temperature, is controlled for 200 DEG C, pressure is from liter pressure；
(7), X-ray is entered from the central axial direction of bonnet 9, and from the longitudinal horn mouth of protecgulum 11 detector is reached.
(8), continuous detector gathers the X-ray signal that diffraction goes out, you can obtain Ti-Si catalyst in synthesis crystallization process
In, its dynamic XRD change information.
Embodiment 2：
All devices are with embodiment 1, concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is soft graphite.The material for determining window 1 and dynamic window 3 is the boron nitride ceramics of X-ray material.
(2) dynamic window seat 7, is rotated, the axial direction size of sample bin 2 is adjusted, light path is 0.1mm on ShiXGuang roads.
(3), sample bin 2 is put into disc-shaped Ni/ZnO catalyst, assembles the continuously adjustable catalyst dynamic structure of light path
In-situ characterization device, bonnet 9 is uniformly distributed 8 large through-holes with protecgulum 12, and bolt is connected bonnet 9 and protecgulum 11 by large through-hole
Fastening.
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 6 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6), connecting fluid inlet pipe 5, outlet pipe 10, the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is connected
In being connected to experimental provision, gas medium hydrogen is passed through；
(7) temperature, is controlled for 400 DEG C, pressure is 6MPa；
(8), X-ray is entered from the central axial direction of bonnet 9, and from the longitudinal horn mouth of protecgulum 11 detector is reached.
(9), the X-ray signal for continuously being gone out with detector acquisition of transmission, you can obtain catalyst during reduction activation, its
Dynamic XAFS change informations.
Embodiment 3：
All devices are with embodiment 1, concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is polytetrafluoroethylene (PTFE).The material for determining window 1 and dynamic window 3 is the polyimides of X-ray material.
(2) dynamic window seat 7, is rotated, the size of the axial direction of sample bin 2 is adjusted, light path is 3mm on ShiXGuang roads.
(3), sample bin 2 is put into disc-shaped Pb/ graphen catalysts, assembles the continuously adjustable catalyst dynamic knot of light path
Structure in-situ characterization device, bonnet 9 is uniformly distributed 4 large through-holes with protecgulum 12, and bolt is connected bonnet 9 and protecgulum 11 by large through-hole
Connect fastening.
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 2 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6), connecting fluid inlet pipe 5, outlet pipe 10, the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is connected
In being connected to experimental provision, gas reaction medium carbon monoxide and oxygen are passed through；
(7) temperature, is controlled for 50 DEG C, pressure is 0.3MPa；
(8), X-ray is entered from the central axial direction of bonnet 9, and from the longitudinal horn mouth of protecgulum 11 detector is reached.
(9), the X-ray signal for continuously being gone out with detector acquisition of transmission, you can obtain Pb/ graphen catalysts in carbon monoxide
In oxidizing process, its dynamic XAFS change information.
Embodiment 4：
All devices are with embodiment 1, concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is polytetrafluoroethylene (PTFE).The material for determining window 1 and dynamic window 3 is metallic beryllium, its surface vapor deposition nitrogen
Change boron.
(2) dynamic window seat 7, is rotated, the axial direction size of sample bin 2 is adjusted, light path is 1mm on ShiXGuang roads.
(3) the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path, is assembled, bonnet 9 is uniform with protecgulum 12
Bonnet 9 and protecgulum 11 are connected fastening by 6 large through-holes of distribution, bolt by large through-hole.By colloidal phosphate aluminium molecular sieve catalyst
Injection sample bin 2, inlet pipe 5, the tail end of outlet pipe 10 are installed through type two and are led to, the general dead stifled sealing of through type two；
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 4 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6) temperature, is controlled for 150 DEG C, pressure is from liter pressure；
(7), X-ray is entered from the longitudinal horn mouth of protecgulum 11 with 1 one-tenth of window, 45 degree of angles are determined, and fluorescence X signal passes through protecgulum
11 longitudinal horn mouth reaches detector.
(8), continuous detector gathers the X-ray signal that diffraction goes out, you can obtain phosphorus Al catalysts in synthesis crystallization process
In, its dynamic XAFS change information.
Embodiment 5：
All devices are with embodiment 1, concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is polytetrafluoroethylene (PTFE).The material for determining window 1 and dynamic window 3 is metallic beryllium, its surface vapor deposition nitrogen
Change boron.
(2) dynamic window seat 7, is rotated, the axial direction size of sample bin 2 is adjusted, light path is 0.8mm on ShiXGuang roads.
(3) the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path, is assembled, bonnet 9 is uniform with protecgulum 12
Bonnet 9 and protecgulum 11 are connected fastening by 6 large through-holes of distribution, bolt by large through-hole.By colloidal phosphate aluminium molecular sieve catalyst
Injection sample bin 2, inlet pipe 5, the tail end of outlet pipe 10 are installed through type two and are led to, the general dead stifled sealing of through type two；
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 4 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6) temperature, is controlled for 180 DEG C, pressure is from liter pressure；
(7), X-ray is entered from the central axial direction of bonnet 9, and from the longitudinal horn mouth of protecgulum 11 detector is reached.
(8), the continuous X-ray signal scattered with detector collection, you can obtain phosphorus Al catalysts in synthesis crystallization process
In, its dynamic SAXS change information.
Embodiment 6：
All devices are with embodiment 1, concrete steps：
(1), select to determine window 1 and determine between window seat 4, between plain cushion ring 6 and dynamic window seat 7, plain cushion ring 6 and rear pressure ring
Sealing gasket material between 8 is polytetrafluoroethylene (PTFE).The material for determining window 1 and dynamic window 3 is the metallic beryllium of X-ray material.
(2) dynamic window seat 7, is rotated, the axial direction size of sample bin 2 is adjusted, light path is 1.2mm on ShiXGuang roads.
(3), sample bin 2 is put into 100～160 mesh Ni/ZnO catalyst, assembles the continuously adjustable catalyst dynamic of light path
Structure in-situ characterization device, bonnet 9 is uniformly distributed 8 large through-holes with protecgulum 12, and bolt passes through large through-hole by bonnet 9 and protecgulum 11
Connection fastening.
(4), it is put into cartridge heater in bonnet 9 and 12 equally distributed 6 small through hole of protecgulum；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6), connecting fluid inlet pipe 5, outlet pipe 10, the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is connected
In being connected to experimental provision, the mould oil containing thiophene of gas medium hydrogen and liquid is passed through；
(7) temperature, is controlled for 280 DEG C, pressure is 3MPa；
(8), X-ray is entered from the central axial direction of bonnet 9, and from the longitudinal horn mouth of protecgulum 11 detector is reached.
(9), the X-ray signal for continuously being gone out with detector acquisition of transmission, you can obtain Ni/ZnO catalyst de- in adsorption reaction
During sulphur, its dynamic XAFS change information.
Claims (16)
1. the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of a kind of light path, it includes determining window (1), sample bin (2),
Dynamic window (3), determines window seat (4), and inlet pipe (5), plain cushion ring (6) moves window seat (7), rear pressure ring (8), bonnet (9), outlet pipe
(10), protecgulum (11), it is characterised in that there is longitudinal horn mouth protecgulum (11) upside, under it is little big, determine window (1) positioned at calmly
Window seat (4) upper surface, dynamic window (3) is embedded in dynamic window seat (7) upper surface, and dynamic window seat (7) axially has through hole, moves window
Seat (7) is interior positioned at window seat (4) is determined, and is threaded connection, and determines window (1), determines shape between window seat (4) and dynamic window (3)
Into sample bin (2), determining window seat (4) has symmetrical 2 axial circular holes, and communicates with sample bin (2), inlet pipe (5), outlet pipe (10) point
Do not communicate with 2 axial circular holes, rear pressure ring (8) has positioned at dynamic window seat (7) lower end between rear pressure ring (8) and dynamic window seat (7)
Plain cushion ring (6), rear pressure ring (8) is connected with fastening with rear wedge (9) with thread connection, bonnet (9) and protecgulum (11).
2. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
4-8 large through-hole is uniformly distributed in described bonnet (9) and protecgulum (12), in bonnet (9) and protecgulum (12) 2-6 is uniformly distributed
Small through hole.
3. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
In it is described determine window (1) and determine between window seat (4), between plain cushion ring (6) and dynamic window seat (7), plain cushion ring (6) and rear pressure ring
(8) there is sealing gasket between.
4. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 3, its feature exists
In the material of the sealing gasket be polytetrafluoroethylene (PTFE), polyimides or soft graphite.
5. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 4, its feature exists
Selected according to experimental temperature in the gasket material, polytetrafluoro, polyimides or soft graphite are selected in temperature≤250 DEG C；
Temperature in 250 DEG C and≤400 DEG C of ＞, from polyimides or soft graphite.
6. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
There is interior hexagonal endoporus in dynamic window seat (7) lower surface.
7. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
In it is described change sample bin (2) axial direction size adjusting range be 0.01～3mm.
8. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
Through type two is installed in the inlet pipe (5) or outlet pipe (10) tail end to lead to.
9. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
There is interior hexagonal endoporus in the lower surface of the rear pressure ring (8).
10. a kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path as claimed in claim 1, its feature exists
Determine window (1), dynamic window (3) and be made up of the metallic beryllium of saturating X-ray material, boron nitride ceramics or polyimides in described.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 11. as claimed in claim 1 light paths, its feature exists
Determine window (1), move the selection metallic beryllium that window (3) is X-ray material in described.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 12. light paths as described in claim 10 or 11, its
It is characterised by the metallic beryllium in its surface vapor cvd nitride boron, aluminum oxide or polyimide film.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 13. light paths as described in claim 10 or 11, its
It is characterised by that metallic beryllium is applied to reducing atmosphere.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 14. light paths as described in claim 10 or 13, its
The metallic beryllium for being characterised by polyimides, boron nitride ceramics or inner surface cvd nitride boron membrane is applied to reproducibility, oxidisability
Or inertia.
A kind of continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 15. light paths as described in any one of claim 1-15
Application, it is characterised in that comprise the steps：
The continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is under the conditions of room temperature～500 DEG C, normal pressure～6MPa
Work, is characterized using XRD and XAFS transmission modes, and when XRD transmission modes are characterized, X-ray enters from the central axial direction of bonnet (9)
Enter, and carry sample message, from the longitudinal horn mouth of protecgulum (11) detector is reached；When XAFS fluorescence modes are characterized, X-ray
Enter into 45 degree of angles with window (1) is determined from the longitudinal horn mouth of protecgulum (11), fluorescence signal also by protecgulum (11) elongated slot
Formula horn mouth reaches detector.
A kind of application of the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of 16. as claimed in claim 15 light paths,
It is characterized in that including that step is as follows including specific detection：
(1), according to the gasket material that choice of experimental conditions is suitable, the material of window (1) and dynamic window (3), seal Backing material are determined
Material is selected according to experimental temperature, and≤250 DEG C are selected polytetrafluoro, polyimides or soft graphite；250 DEG C of ＞ and≤400
DEG C from polyimides or soft graphite, determine the material of window 1 and dynamic window 3 according to experiment atmosphere selection, metallic beryllium is applied to
Reducing atmosphere, the metallic beryllium of polyimides, boron nitride ceramics or inner surface cvd nitride boron membrane is applied to reproducibility, oxidation
Property or inert atmosphere；
(2), in the range of 0.01～3mm, dynamic window seat (7) of rotation adjusts the size of sample bin (2) axial direction to suitable chi
It is very little；
(3), first by solid-state testing sample loading sample bin (2), refill and prepare the continuously adjustable catalyst dynamic structure original of light path
Position characterization apparatus；Or the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is first assembled, then liquid sample is noted
Enter sample bin (2)；
(4) heater element and temperature control galvanic couple, are placed；
(5), the continuously adjustable representing characteristics of normal position of dynamic catalyst structure device of light path is put into X-ray road, and is fixed；
(6), connecting fluid inlet pipe (5), outlet pipe (10), sample cell is connected in experimental provision；
(7), in room temperature～500 DEG C, between normal pressure～6MPa, the actual response condition according to required for being characterized catalyst sets
Determine temperature and pressure；
(8) when, using XRD modelings, X-ray is entered from the central axial direction of bonnet (9), and carries sample message, from protecgulum
(11) longitudinal horn mouth reaches detector；When being characterized using XAFS fluorescence modes, longitudinal loudspeaker of the X-ray from protecgulum (11)
Mouth is entered with 1 one-tenth of window, 45 degree of angles are determined, and fluorescence signal reaches detector also by the longitudinal horn mouth of protecgulum (11)；
(9) X-ray signal, scattering that, the X-ray signal of the detector acquisition of transmission for persistently being provided with Synchrotron Radiation, diffraction go out
The X-ray signal for going out, you can obtain catalyst in experimentation, the change information of its structure dynamics.
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