CN103728247A - In-situ gas-solid phase reaction pool for measuring high-temperature high-pressure dynamic field spectrum in situ - Google Patents
In-situ gas-solid phase reaction pool for measuring high-temperature high-pressure dynamic field spectrum in situ Download PDFInfo
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- CN103728247A CN103728247A CN201410003940.6A CN201410003940A CN103728247A CN 103728247 A CN103728247 A CN 103728247A CN 201410003940 A CN201410003940 A CN 201410003940A CN 103728247 A CN103728247 A CN 103728247A
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Abstract
The invention provides an in-situ gas-solid phase reaction pool for measuring high-temperature high-pressure dynamic field spectrum in situ. The reaction pool comprises a heating stage main body and an internal sample pool, wherein one side of the heating stage main body is provided with an air inlet passage, a reaction pool cover is arranged above the heating stage main body, and is provided with an unthreaded hole, and a window plate covers the unthreaded hole. The internal lower part of the heating stage main body is provided with a cabin body space for storing the sample pool, the bottom of the heating stage main body is provided with a horizontal adjusting transmission rod and is connected with the sample pool in the reaction pool cavity, the sample pool can move on the horizontal plane, a heating wire is wound at the periphery of the pool body, a thermocouple is inserted into the pool body, the bottom of the pool body is provided with an air outlet, and a cooling water passage is respectively arranged in each of the heating stage main body and the reaction pool cover. As a heating state adopts an internal adjusting way, the size of the unthreaded hole is reduced, the thickness of a quartz plate is reduced, the signal attenuation is reduced, a high space resolution requirement is met, and the structural variation of the sample can be monitored under the high-temperature high-pressure reaction condition.
Description
Technical field
The invention belongs to instrument analysis technology field, particularly the dynamic on-the-spot In situ spectroscopic gas-solid phase reaction measurement reaction tank of a kind of High Temperature High Pressure.
Background technology
High Temperature High Pressure gas-solid-phase catalytic reaction is the common reaction type of chemical industry.Under reaction conditions, absorption, reaction, the desorption of gas on solid sample is the important step of gas-solid phase or heterogeneous catalysis, the structural change of the molecular structure of solid sample under reaction conditions itself is the formation that discloses catalyst active center, the key issue of reacting structure-effect relationship and catalyst deactivation.
Modern molecular spectroscopy techniques is all widely used in the fields such as physics, chemistry, biology.Take Raman spectrum as example, and its off-line characterization research in solid catalyst powdered sample structure has also been carried out much work.Existing Raman spectrum reaction tank, although can carry out the research of temperate condition (atmospheric low-temperature) original position, considers the requirement of pressure to window thickness, reacting system pressure is higher, window thickness is larger, thereby add high attenuation, surveys light intensity, and loss derives from the Raman signal of sample.Therefore, also not having at present can be under harsh conditions (temperature: 300～1000 ℃, pressure: 10-100 kilogram) effective Study of Catalyst reaction tank.
Summary of the invention
For the defect of prior art, the invention provides and a kind ofly can under High Temperature High Pressure, carry out the reaction tank of original position sample detection, can be used for comprising all dynamic on-the-spot In situ spectroscopic research of Raman spectrum.
A kind of gas-solid phase reaction in-situ pond, it is characterized in that, described reaction tank comprises: a unthreaded hole 11 with quartzy window 21 is positioned at the middle part of reaction tank lid 1, is provided with cooling-water duct 22 and is connected with the cooling water outlet and inlet 10 that reaction tank covers on 1 sidewall in reaction tank lid 1; An Intermediate Gray has the reaction tank main body 7 of cavity 12, columniform sample cell 3 is placed in cavity 12, the outer wall of sample cell 3 is provided with heating wire 18, its upper end has a circle thin slice and carries groove 16, centre arranges a sample cell outlet passageway 17 and is communicated with the sample cell venthole 23 of bottom, the first adjuster bar 5 and the second adjuster bar 6 stretch in cavity 12 through reaction tank main body 7, its front end is connected with the second draw-in groove 14 with the first draw-in groove 13 of sample cell bottom by reaction tank adjusting part 4, and the tail end of the first adjuster bar 5 and the second adjuster bar 6 arranges adjusting screw thread; Reaction tank main body 7 inside are provided with reaction tank cooling-water duct 20, are connected with the reaction tank cooling-water duct mouth 24 that is positioned at reaction tank main body outer wall, are also provided with air admission hole 9 and venthole 8 on reaction tank main body outer wall; Reaction tank lid 1 is connected in reaction tank main body 7, between reaction tank lid 1 and reaction tank main body 7, is provided with O RunddichtringO 2.
The material of described sample cell 3 is a kind of in stainless steel, pottery, corundum.
The diameter of described unthreaded hole 11 is footpath 2-5mm.
Described quartzy window is that thickness is the ultraviolet fused quartz window of 0.5-2.0mm.
It is 5-20mm that described thin slice carries groove diameter, and the degree of depth is 0.5-3mm.
Beneficial effect
The invention has the advantages that:
(1) above sample cell, have thin slice and carry groove, can to powder or thin slice sample, carry out the measurement of In situ spectroscopic as required.
(2) sample cell can carry out translation in the body internal water plane of reaction tank cabin, both reduced the required size of unthreaded hole, reduce again the thickness of the quartzy window of unthreaded hole, thereby reduce the signal being caused by window thickness, reduce and disturb, can realize the statistical rule of the structural change of sample under High Temperature High Pressure.
Accompanying drawing explanation
Fig. 1 is reaction in-situ pond broken away view.
Wherein, 1: reaction tank lid, 2:O RunddichtringO, 3: sample cell, 4: reaction tank adjusting part, 5: the first adjuster bars, 6: the second adjuster bars, 7: reaction tank main body, 8: reaction tank venthole, 9: reaction tank air admission hole, 10: reaction tank lid cooling-water duct mouth, 11: unthreaded hole, 12: reaction tank cavity, 13: the first draw-in grooves, 14: the second draw-in grooves, 15: motion thread, 16: thin slice carries groove, 17: sample cell outlet passageway, 18: heater strip, 19: temperature control passage, 20: reaction tank cooling-water duct, 21: quartzy window, 22: reaction tank lid cooling-water duct, 23: sample cell venthole, 24: reaction tank cooling-water duct mouth, 25: heater strip passage, 26: adjuster bar penetrates hole.
Fig. 2 is vertical view (a), cross-section front view (b), cross sectional side view (c) and the oblique side view (d) of reaction tank top cover.
Wherein, 1: reaction tank lid, 10: reaction tank lid cooling-water duct mouth, 11: unthreaded hole, 21: quartzy window, 22: reaction tank lid cooling-water duct.
Fig. 3 is upward view (a), cross-sectional view (b, d), vertical view (c) and the oblique side view (e) of sample cell and adjuster bar.
Wherein, 3: sample cell, 5: the first adjuster bars, 13: the first draw-in grooves of 6: the second adjuster bars, 14: the second draw-in grooves, 15: motion thread, 16: thin slice carries groove, 17: sample cell outlet passageway, 18: heater strip, 23: sample cell outlet passageway mouth.
Fig. 4 is vertical view (a), side view (b), cross-section front view (c) and the oblique side view (d) of reaction tank main body.
Wherein, 8: reaction tank venthole, 9: reaction tank air admission hole, 12: reaction tank cavity, 19: temperature control passage, 20: reaction tank cooling-water duct, 24: reaction tank cooling-water duct mouth, 25: heater strip passage, 26: adjuster bar penetrates hole.
Fig. 5 is the situ high pressure Raman spectrum (H of di-iron trioxide reduction process
2flow: 20ml/min).
Embodiment
Reaction tank of the present invention covers and has unthreaded hole, is furnished with quartzy window.Reaction tank main body has inlet channel, and inside is provided with the cabin body space of placing sample cell.Sample cell is connected with adjuster bar with draw-in groove by adjusting part, by the transmission of screw thread, reaches the movement of sample cell on surface level, thereby reaches spatial discrimination.Sample cell bottom has venthole, and goes out gas piping and is connected.Sample cell is built-in with heater element and thermopair, realizes temperature and controls and measure.Reaction tank main body and reaction tank lid is equipped with cooling-water duct, guarantees not temperature influence and being out of shape of pond body, increases the service life.
Sample cell of the present invention is bottom opening, and top has the cylinder that thin slice carries groove, and material is stainless steel, pottery or corundum.Feature is according to demand, to powdered sample and moulding sheet sample, to carry out raman spectroscopy.
Below in conjunction with drawings and Examples, the invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment
High Temperature High Pressure gas-solid phase raman response pond as shown in Figure 1, Figure 2, Figure 3 and Figure 4.Reaction tank main body and reaction tank lid material are stainless steel, and body interior and top cover inside all have bosh, and main body also has into outlet passageway and temperature control passage, concrete size is as follows: main diameter is 59mm, high 20mm, inner sample pool space size diameter is 24mm, dark 16mm.Sample cell external diameter 14mm, internal diameter 10mm, dark 5mm, thin slice carries groove diameter 12mm, dark 1mm.Sealing O type circle external diameter is 43.5mm, internal diameter 38.5mm.Quartzy window diameter 17mm, thick 1mm, unthreaded hole diameter is 3mm.In example, adjuster bar stretches in cavity through reaction tank main body, by adjusting part, be connected with sample cell with sample cell draw-in groove, the kind of drive adopts screw thread transmission, sample upper end has thin slice and carries groove, between reaction tank top cover and main body, add O-ring seal, by 8 screws, connect and seal (also can connect by flange).
In this example, with the commercial Fe of Aladdin reagent company
2o
3for powdered sample, first sample cell heelpiece last layer silica wool, after sample is filled in sample cell, with flat-top glass bar, by sample compacting, and clear up smoothly, cover reaction tank lid and O type packing ring, with screw and nut, reaction cabin is sealed.Then reaction tank is fixed in detection platform, adjustable lens and position of platform, regulate sample cell position, makes Laser Focusing on sample.Air inlet is connected with outside gas circuit with gas outlet, passes into H
2, regulate pressure, adopt spectrum in good time, see Fig. 5.In Fig. 5, sample first, under the condition of not coupled reaction Chi Gai, scans Raman spectrum; Then cover top cover sealing, at normal temperatures, in hydrogen environment, under different pressures, scanning Raman spectrum; When pressure rises to after 5Mpa, under different temperatures, scanning Raman spectrum; When pressure rises to 5Mpa, temperature rises to after 350 ℃, stablizes different time, scanning Raman spectrum; Under the same conditions, regulate sample cell position finally, scan the Raman spectrum of different sample spot.
The present invention adopts sample cell in the inner mobile mode of reaction tank, has reduced unthreaded hole diameter and window thickness, has solved under high pressure because window thickness increases, thereby has caused problem of signal attenuation.By instance graph 5 results, can be found out, under same test condition, in reaction tank, the test result of sample is compared with the result of direct Raman test, although signal weakens to some extent, but guaranteed the collection of sample signal, and realized the raman spectroscopy measurement of reaction pressure under 0.1～5Mpa, the actual response condition of temperature of reaction at 20～350 ℃, meanwhile, realized multi-point sampler, thereby got rid of the possibility of long-time irradiating laser to the damage influence result of sample, also can obtain the statistical rule of sample different sample spot under High Temperature High Pressure.
Claims (5)
1. a gas-solid phase reaction in-situ pond, it is characterized in that, described reaction tank comprises: a unthreaded hole with quartzy window (21) (11) is positioned at the middle part of reaction tank lid (1), is provided with cooling-water duct (22) and is connected with the cooling water outlet and inlet (10) on reaction tank lid (1) sidewall in reaction tank lid (1), an Intermediate Gray has the reaction tank main body (7) of cavity (12), columniform sample cell (3) is placed in cavity (12), the outer wall of sample cell (3) is provided with heating wire (18), its upper end has a circle thin slice and carries groove (16), centre arranges a sample cell outlet passageway (17) and is communicated with the sample cell venthole (23) of bottom, the first adjuster bar (5) and the second adjuster bar (6) stretch in cavity (12) through reaction tank main body (7), its front end is connected with the second draw-in groove (14) with first draw-in groove (13) of sample cell bottom by reaction tank adjusting part (4), the tail end of the first adjuster bar (5) and the second adjuster bar (6) arranges adjusting screw thread, reaction tank main body (7) inside is provided with reaction tank cooling-water duct (20), be connected with the reaction tank cooling-water duct mouth (24) that is positioned at reaction tank main body outer wall, on reaction tank main body outer wall, be also provided with air admission hole (9) and venthole (8), it is upper that reaction tank lid (1) is connected to reaction tank main body (7), between reaction tank lid (1) and reaction tank main body (7), is provided with O RunddichtringO (2).
2. a gas-solid phase reaction in-situ as claimed in claim 1 pond, is characterized in that, the material of described sample cell (3) is a kind of in stainless steel, pottery, corundum.
3. a gas-solid phase reaction in-situ as claimed in claim 1 pond, is characterized in that, the diameter of described unthreaded hole (11) is 2-5mm.
4. a gas-solid phase reaction in-situ as claimed in claim 1 pond, is characterized in that, described quartzy window is that thickness is the ultraviolet fused quartz window of 0.5-2.0mm.
5. a gas-solid phase reaction in-situ as claimed in claim 1 pond, is characterized in that, it is 5-20mm that described thin slice carries groove diameter, and the degree of depth is 0.5-3mm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124408A (en) * | 2016-06-16 | 2016-11-16 | 华东理工大学 | A kind of condensation-proof type reactor for the test of dynamic field In situ spectroscopic |
| CN106198390A (en) * | 2016-08-09 | 2016-12-07 | 华东理工大学 | A kind of pollution-proof high-temperature high-pressure dynamic field In situ spectroscopic test reactor |
| CN106290302A (en) * | 2016-08-09 | 2017-01-04 | 华东理工大学 | A kind of self-cleaning high-temperature high-pressure dynamic field In situ spectroscopic test reactor |
| CN107449651A (en) * | 2017-08-03 | 2017-12-08 | 核工业北京地质研究院 | Laser pool device for laser sample preparation mass spectrum oxygen isotope composition analysis |
| CN109540870A (en) * | 2019-01-15 | 2019-03-29 | 大连齐维科技发展有限公司 | Confocal laser-scanning microscopy instrument reaction tank |
| CN109827933A (en) * | 2019-03-12 | 2019-05-31 | 余姚市浙江大学机器人研究中心 | Transition detection device under a kind of high pressure |
| CN110967301A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN113318683A (en) * | 2021-05-12 | 2021-08-31 | 华东理工大学 | Multifunctional low dead volume gas-solid phase reactor suitable for multiple in-situ spectral characterization |
| CN115869858A (en) * | 2023-02-13 | 2023-03-31 | 中国科学技术大学 | High-temperature gas-solid in-situ sum frequency spectrum reaction tank |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124408B (en) * | 2016-06-16 | 2019-03-05 | 华东理工大学 | A kind of condensation-proof type reactor for the test of dynamic field In situ spectroscopic |
| CN106124408A (en) * | 2016-06-16 | 2016-11-16 | 华东理工大学 | A kind of condensation-proof type reactor for the test of dynamic field In situ spectroscopic |
| CN106290302B (en) * | 2016-08-09 | 2019-05-17 | 华东理工大学 | Reactor is used in a kind of test of self-cleaning high-temperature high-pressure dynamic field In situ spectroscopic |
| CN106198390A (en) * | 2016-08-09 | 2016-12-07 | 华东理工大学 | A kind of pollution-proof high-temperature high-pressure dynamic field In situ spectroscopic test reactor |
| CN106290302A (en) * | 2016-08-09 | 2017-01-04 | 华东理工大学 | A kind of self-cleaning high-temperature high-pressure dynamic field In situ spectroscopic test reactor |
| CN106198390B (en) * | 2016-08-09 | 2018-10-26 | 华东理工大学 | A kind of pollution-proof high-temperature high-pressure dynamic field In situ spectroscopic test reactor |
| CN107449651A (en) * | 2017-08-03 | 2017-12-08 | 核工业北京地质研究院 | Laser pool device for laser sample preparation mass spectrum oxygen isotope composition analysis |
| CN110967301A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN110967301B (en) * | 2018-09-29 | 2023-10-03 | 中国科学院大连化学物理研究所 | In-situ sum frequency vibration spectrum detection device with laser heating function |
| CN109540870A (en) * | 2019-01-15 | 2019-03-29 | 大连齐维科技发展有限公司 | Confocal laser-scanning microscopy instrument reaction tank |
| CN109827933A (en) * | 2019-03-12 | 2019-05-31 | 余姚市浙江大学机器人研究中心 | Transition detection device under a kind of high pressure |
| CN109827933B (en) * | 2019-03-12 | 2021-08-10 | 余姚市浙江大学机器人研究中心 | Phase transition state detection device under high pressure |
| CN113318683A (en) * | 2021-05-12 | 2021-08-31 | 华东理工大学 | Multifunctional low dead volume gas-solid phase reactor suitable for multiple in-situ spectral characterization |
| CN115869858A (en) * | 2023-02-13 | 2023-03-31 | 中国科学技术大学 | High-temperature gas-solid in-situ sum frequency spectrum reaction tank |
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Application publication date: 20140416 |