CN103084127A - High-temperature normal-pressure catalytic reactor suitable for mass spectrometry and application thereof - Google Patents
High-temperature normal-pressure catalytic reactor suitable for mass spectrometry and application thereof Download PDFInfo
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- CN103084127A CN103084127A CN2013100231355A CN201310023135A CN103084127A CN 103084127 A CN103084127 A CN 103084127A CN 2013100231355 A CN2013100231355 A CN 2013100231355A CN 201310023135 A CN201310023135 A CN 201310023135A CN 103084127 A CN103084127 A CN 103084127A
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Abstract
The invention discloses a high-temperature normal-pressure catalytic reactor suitable for mass spectrometry and an application thereof. The reactor consists of a furnace body, a sample introduction pipe, a high-temperature catalyst chamber, a reaction area, a difference hole, a micropore and an air outlet pipe. When samples react in the reaction area, the sample introduction pipe is continuously inflated, the reaction area can maintain to be in a normal-pressure state, and the samples can be subjected to catalytic reaction at different temperatures by adjusting the temperature of the high-temperature catalyst chamber to generate catalysates, free radicals and intermediates, and then catalysates, the free radicals and the intermediates spread towards an ionization chamber by the micropore under the action of pressure and form a molecular beam after passing through the difference hole to enter a mass spectrum ionization chamber, thus solving the problem that the free radicals and the unstable intermediates are difficult to detect in situ during the normal-pressure catalytic reaction.
Description
Technical field
The present invention relates to a kind of catalyst furnace field, be specifically related to a kind of high-temperature pressure catalytic reaction stove and application of suitable mass spectral analysis.
Background technology
The chemical reaction that carries out under catalyst action is called catalytic reaction.In chemical reaction, original some chemical bond of reaction molecular must dissociate and form new chemical bond, and this needs certain activation energy.In some is difficult to the system of chemical reaction occurs, add the third material (catalyst) that helps the reaction molecular chemical bond to reset, its effect can reduce the activation energy of reaction, thereby can accelerate the selective and stereospecificity of chemical reaction and control product.In catalytic reaction process, the rearrangement of new chemical bond will produce a series of novel substance, free radical and intermediate, to the research of catalytic process and product help the to promote mutual understanding structure and composition of material, can help to analyze the catalysis behavior to the impact of whole course of reaction, therefore, the catalytic process of fully realizing material can further be illustrated the molecular structure of material.
Mass-spectrometric technique is a kind of analytical method of measuring the ion charge-mass ratio, and its principle is to make that in sample, each component ionizes in ion gun, generates the positively charged ion of different charge-mass ratios, through the effect of accelerating field, forms ion beam, enters mass analyzer.In mass analyzer, the recycling Electric and magnetic fields makes opposite velocity dispersion occurs, and they are focused on respectively and obtains mass spectrogram, thereby determine its quality.Mass-spectrometric technique commonly used has level Four bar mass spectrum, ion trap mass spectrometry, flight time mass spectrum etc. at present.Wherein level Four bar mass spectrum is the ion that utilizes different quality, and the difference of movement locus is analyzed by measured ion in radiofrequency field; Ion trap mass spectrometry is to distinguish the quality of ion by different ions restraint conditions difference in ion trap; Flight time mass spectrum is by after giving identical energy, and fast these characteristics of the ion flight that ion flight speed is slow, quality is little that quality is large are measured the quality of ion.
At present, the pressure in catalytic reaction mostly is greatly normal pressure and high pressure conditions, and also mostly for the analysis of catalysate is to adopt first to collect catalysate, determines stable product component by chromatogram or mass spectral analysis.But the free radical that produces in course of reaction and intermediate just easily react with other materials in normal pressure and transmitting procedure, therefore utilize appeal method can't obtain in real time, accurately the to be correlated with dynamic information of catalytic reaction process.The present invention will solve that in the normal pressure catalytic reaction, free radical and unstable intermediate are difficult to by the problem of in situ detection.
Summary of the invention
The defective that exists in order to overcome prior art the purpose of this invention is to provide a kind of high-temperature pressure catalytic reaction stove and application of suitable mass spectral analysis, the free radical and the intermediate that produce in catalytic process for detection of sample.Its design philosophy is to add an escape pipe in the catalytic reaction zone rear end, and constantly inflation in sample feeding pipe, gas is discharged by escape pipe by reaction zone, namely forms a loop, guarantees that reaction zone keeps atmospheric pressure state; In addition the catalytic reaction stove is directly fixed on the front end of mass spectrum ionisation chamber, when material generation catalytic reaction, by regulating the temperature of high-temperature catalytic chamber, make material under different temperatures, catalytic reaction occur, product is because pressure-acting spreads to the mass spectrum ionisation chamber, when entering ionisation chamber through forming molecular beam behind the difference hole, by the mass spectrum in situ detection.
The invention provides a kind of high-temperature pressure catalytic reaction stove of suitable mass spectral analysis, this reacting furnace comprises body of heater, sample feeding pipe, high-temperature catalytic chamber, reaction zone, difference hole, micropore and escape pipe; The high-temperature catalytic chamber is at the body of heater center, and reaction zone is in the high-temperature catalytic chamber interior, and the reaction zone front end is connected with sample feeding pipe, and the reaction zone rear end connects tracheae, and opens a micropore, and the micropore rear end is the difference hole; Sample feeding pipe, micropore and center, difference hole keep in the same horizontal line; When sample reacts in reaction zone, make sample under different temperatures, catalytic reaction occur by the temperature of regulating the high-temperature catalytic chamber, catalysate, free radical and intermediate be because pressure-acting sees through micropore to the diffusion of mass spectrum ionisation chamber, when entering the mass spectrum ionisation chamber through forming molecular beam behind the difference hole; Reaction constantly to the sample feeding pipe inflation, makes reaction zone keep atmospheric pressure state simultaneously.
The high-temperature pressure catalytic reaction stove of suitable mass spectral analysis provided by the invention, described sample feeding pipe and escape pipe are fused quartz tube, and external diameter is 6mm, and internal diameter is 4mm.The aperture in described difference hole is 0.5mm, and material is quartzy.Described micropore size is 0.1mm, adopts the laser boring mode.Described reaction zone is normal pressure.
The high-temperature pressure catalytic reaction stove of suitable mass spectral analysis provided by the invention, the temperature of described reacting furnace and pressure are by high-temperature catalytic chamber control; The temperature of high-temperature catalytic chamber can reach 1200 ℃ of left and right; The pressure of high-temperature catalytic chamber controls by lobe pump and reaches 1 ~ 300Pa.
The present invention also provides the application of the high-temperature pressure catalytic reaction stove of described suitable mass spectral analysis, and this reacting furnace is applied to heterogeneous catalytic reaction; Wherein gas reactant adopts the mass flowmenter sample introduction, and solid catalyst adopts direct sintering in sample feeding pipe, and liquid reactants adopts the bubbling input mode.
The invention has the beneficial effects as follows: the present invention makes catalytic reaction occur in atmospheric pressure state, makes simultaneously the catalysate very first time enter the ionization of mass spectrum ionisation chamber, by the mass spectrum in situ detection.
Description of drawings
Fig. 1 is the structural representation of the high-temperature pressure catalytic reaction stove of a kind of suitable mass spectral analysis of the present invention; Wherein (1) is body of heater, and (2) are sample feeding pipe, and (3) are the high-temperature catalytic chamber, and (4) are reaction zone, and (5) are the difference hole, and (6) are micropore, and (7) are escape pipe;
Fig. 2 is take flight time mass spectrum as example, high-temperature pressure catalytic reaction stove and flight time mass spectrum connection diagram.Wherein (8) are high-temperature pressure catalytic reaction stove, and (9) are flight time mass spectrum.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention is described in further details.
As shown in Figure 1, the high-temperature pressure catalytic reaction stove of a kind of suitable mass spectral analysis of the present invention comprises body of heater, sample feeding pipe, high-temperature catalytic chamber, reaction zone, difference hole, micropore and escape pipe.When sample reacts in reaction zone, make sample under different temperatures, catalytic reaction occur by the temperature of regulating the high-temperature catalytic chamber, catalysate, free radical and intermediate spread to ionisation chamber because pressure-acting sees through micropore, when entering the mass spectrum ionisation chamber through forming molecular beam behind the difference hole.Reaction constantly to the sample feeding pipe inflation, makes reaction zone keep atmospheric pressure state simultaneously.
The present invention can be applied to the analysis of catalysate free radical and intermediate under high-temperature pressure, utilization adds an escape pipe in the catalytic reaction zone rear end, and constantly inflation in sample feeding pipe, gas is discharged by escape pipe by reaction zone, namely form a loop, guarantee that reaction zone keeps atmospheric pressure state; In addition catalyst furnace is directly fixed on the front end of mass spectrum ionisation chamber, when material generation catalytic reaction, by regulating the temperature of high-temperature catalytic chamber, make material under different temperatures, catalytic reaction occur, product is because pressure-acting spreads to the mass spectrum ionisation chamber, when entering ionisation chamber through forming molecular beam behind the difference hole, by the mass spectrum in situ detection.
Claims (9)
1. the high-temperature pressure catalytic reaction stove of a suitable mass spectral analysis is characterized in that: this reacting furnace comprises body of heater, sample feeding pipe, high-temperature catalytic chamber, reaction zone, difference hole, micropore and escape pipe;
The high-temperature catalytic chamber is at the body of heater center, and reaction zone is in the high-temperature catalytic chamber interior, and the reaction zone front end is connected with sample feeding pipe, and the reaction zone rear end connects tracheae, and opens a micropore, and the micropore rear end is the difference hole; Sample feeding pipe, micropore and center, difference hole keep in the same horizontal line;
When sample reacts in reaction zone, make sample under different temperatures, catalytic reaction occur by the temperature of regulating the high-temperature catalytic chamber, catalysate, free radical and intermediate be because pressure-acting sees through micropore to the diffusion of mass spectrum ionisation chamber, when entering the mass spectrum ionisation chamber through forming molecular beam behind the difference hole; Reaction constantly to the sample feeding pipe inflation, makes reaction zone keep atmospheric pressure state simultaneously.
2. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: described sample feeding pipe and escape pipe are fused quartz tube, and external diameter is 6mm, and internal diameter is 4mm.
3. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: the aperture in described difference hole is 0.5mm, and material is quartzy.
4. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: described micropore size is 0.1mm, adopts the laser boring mode.
5. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: described reaction zone is normal pressure.
6. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: the temperature of described reacting furnace and pressure are by high-temperature catalytic chamber control.
7. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 6, it is characterized in that: the temperature of described high-temperature catalytic chamber can reach 1200 ℃ of left and right.
8. according to the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 7, it is characterized in that: the pressure of described high-temperature catalytic chamber controls by lobe pump and reaches 1 ~ 300Pa.
9. the application of the high-temperature pressure catalytic reaction stove of the described suitable mass spectral analysis of claim 1, it is characterized in that: this reacting furnace is applied to heterogeneous catalytic reaction; Wherein gas reactant adopts the mass flowmenter sample introduction, and solid catalyst adopts direct sintering in sample feeding pipe, and liquid reactants adopts the bubbling input mode.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN109142503A (en) * | 2018-08-23 | 2019-01-04 | 厦门大学 | A kind of mass spectrometry detection device in situ for heterogeneous catalytic reaction intermediate and product |
| CN109847655A (en) * | 2019-03-08 | 2019-06-07 | 中国科学技术大学 | A kind of experimental provision for in-situ investigation high pressure gas and solid phase catalyzing reaction product |
| CN110208451A (en) * | 2019-04-26 | 2019-09-06 | 合肥工业大学 | Bipolar micro fixed-bed reactor combination Photoionization Mass Spectrometry on-line detecting system and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626412A (en) * | 1984-12-14 | 1986-12-02 | Monsanto Company | Method and apparatus for carrying out catalyzed chemical reactions and for studying catalysts |
| EP1724574A1 (en) * | 2004-02-27 | 2006-11-22 | Japan Science and Technology Agency | Analytical method and analyzer capable of substantially simultaneously analyzing absorption/emission/scattering spectrum and mass spectrum, and analytical method and mass spectroscope utilizing electrospray ionization technique |
| CN101634651A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院大连化学物理研究所 | Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance |
| CN201876386U (en) * | 2010-11-23 | 2011-06-22 | 北京汇丰隆经济技术开发有限公司 | Device for cracking bioaerosol mass spectrum at high temperature |
| CN102359986A (en) * | 2011-07-05 | 2012-02-22 | 中国科学院过程工程研究所 | In-situ detection device and detection method for heat conversion reaction process of solid fuel |
-
2013
- 2013-01-22 CN CN2013100231355A patent/CN103084127A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626412A (en) * | 1984-12-14 | 1986-12-02 | Monsanto Company | Method and apparatus for carrying out catalyzed chemical reactions and for studying catalysts |
| EP1724574A1 (en) * | 2004-02-27 | 2006-11-22 | Japan Science and Technology Agency | Analytical method and analyzer capable of substantially simultaneously analyzing absorption/emission/scattering spectrum and mass spectrum, and analytical method and mass spectroscope utilizing electrospray ionization technique |
| CN101634651A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院大连化学物理研究所 | Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance |
| CN201876386U (en) * | 2010-11-23 | 2011-06-22 | 北京汇丰隆经济技术开发有限公司 | Device for cracking bioaerosol mass spectrum at high temperature |
| CN102359986A (en) * | 2011-07-05 | 2012-02-22 | 中国科学院过程工程研究所 | In-situ detection device and detection method for heat conversion reaction process of solid fuel |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN105784917B (en) * | 2014-12-26 | 2018-06-29 | 中国科学院大连化学物理研究所 | Application of the mass spectrograph during detection is catalyzed reactive ion intermediate |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN107576717B (en) * | 2017-10-24 | 2019-10-25 | 中国科学技术大学 | A kind of in-situ detector being catalyzed reaction gas phase intermediate product for different diffusion lengths |
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN109142503A (en) * | 2018-08-23 | 2019-01-04 | 厦门大学 | A kind of mass spectrometry detection device in situ for heterogeneous catalytic reaction intermediate and product |
| CN109142503B (en) * | 2018-08-23 | 2020-10-16 | 厦门大学 | In-situ mass spectrometry detection device for heterogeneous catalytic reaction intermediate and product |
| CN109847655A (en) * | 2019-03-08 | 2019-06-07 | 中国科学技术大学 | A kind of experimental provision for in-situ investigation high pressure gas and solid phase catalyzing reaction product |
| CN109847655B (en) * | 2019-03-08 | 2024-01-05 | 中国科学技术大学 | Experimental device for be used for normal position to survey high-pressure gas-solid phase catalytic reaction product |
| CN110208451A (en) * | 2019-04-26 | 2019-09-06 | 合肥工业大学 | Bipolar micro fixed-bed reactor combination Photoionization Mass Spectrometry on-line detecting system and method |
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Application publication date: 20130508 |