CN206292192U - Liquid nuclear-magnetism automatic in-situ response analysis test system - Google Patents
Liquid nuclear-magnetism automatic in-situ response analysis test system Download PDFInfo
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- CN206292192U CN206292192U CN201621368678.6U CN201621368678U CN206292192U CN 206292192 U CN206292192 U CN 206292192U CN 201621368678 U CN201621368678 U CN 201621368678U CN 206292192 U CN206292192 U CN 206292192U
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Abstract
The utility model discloses a kind of liquid nuclear-magnetism automatic in-situ response analysis test system, including reaction in-situ unit in liquid superconduction nuclear magnetic resonance spectrometer, chamber, agitating unit and control unit are transmitted outside chamber；In chamber reaction in-situ unit include be nested reactor, be nested reactor locking cap and action separation rotor；The reactor that is nested includes quartz tubular reactor and position internal layer mozzle in the inner；The reactor locking cap that is nested includes that the outer tube locking cap that is enclosed within outside quartz tubular reactor, one end are connected the locking inner core that the other end is connected with inner tube locking cap and is enclosed within internal layer mozzle and the pipeline locking cap that is nested being connected with inner tube locking cap with outer tube locking cap；Action separation rotor includes rotor body, and rotor body is connected by acting release bearing with locking bushing；Agitating unit and control unit are transmitted outside chamber it is connected with reaction in-situ unit in chamber and plays control action.The utility model solves the problems, such as to carry out reaction process synchronization in-situ study in nuclear magnetic resonance cavity.
Description
Technical field
The utility model is related to a kind of liquid nuclear-magnetism automatic in-situ response analysis test system, and specifically one kind can be with
The in-situ characterization analysis system with chemical reaction course under liquid superconduction nuclear magnetic resonance spectrometer on-line checking different condition is realized, is
The functions expanding of the reaction in-situ monitoring realized in traditional liquid superconduction nuclear magnetic resonance spectrometer.
Background technology
Nuclear magnetic resonance spectroscopy（Nuclear Magnetic Resonance Spectroscopy, NMR）NMR is research
Atomic nucleus is to radio-frequency radiation（Radio-frequency Radiation）Absorption, it be to it is various organic and inorganic matter into
Divide, structure carries out one of most strong instrument of qualitative analysis.In nuclear magnetic resonance, there is the interaction of many nuclear spins,
Each may all include abundant structure and dynamic information, add can quantitative analysis, to sample nondestructive wound and can
For specific atom（Core）The features such as, nuclear magnetic resonance is turned into a kind of very good powerful analysis means.Nuclear magnetic resonance
The information of molecule space stereochemical structure is provided, is the important means of analyzing molecules structure and research chemical kinetics.Led in chemistry
Domain, nuclear magnetic resonance provides the effective way of understanding outfield for chemist.
In situNMR（in situ NMR）Refer to that chemical reaction and time Relationship are studied with the method for nuclear magnetic resonance
A kind of research method, it is convenient that the method has, and the characteristics of fast do not destroy reaction system, the research can provide reaction system
In instant data, and reaction in possible transition state information.The application of In situNMR technology for the reaction mechanism mechanism of reaction understanding with
And Catalyst Design transformation provides important theoretical direction data.
Current reaction in-situ research method is in vitro to be added to reactant order in liquid superconduction nuclear magnetic resonance spectrometer
In nuclear magnetic tube, place into liquid superconduction nuclear magnetic resonance spectrometer cavity and detected, if necessary to be divided the whole reaction mechanism mechanism of reaction
Time point is detected, then takes compartment decimation in time reaction solution is detected from reaction vessel method to complete.This method
In the presence of obvious defect：1）It is loaded outside liquid superconduction nuclear magnetic resonance spectrometer cavity, chamber vivo detection, the instantaneity of detection not enough makes
The data that must be obtained are delayed and distortion significantly；2）Extracted from reaction vessel, can cause reaction system impacted so that reactant
The homogeneity of system can not be guaranteed.Therefore, how to develop a kind of on the basis of existing liquid superconduction nuclear magnetic resonance spectrometer
The In situNMR detecting system for being loaded and reacting can be completed in liquid superconduction nuclear magnetic resonance spectrometer cavity, can be met
Monitoring to reaction process, the detection to possible intermediate product.This has turned into current research chemist and has urgently expected to solve
Technical problem, either from research angle or the market demand angle it is all significant.
Utility model content
The utility model cannot be timed sample-adding in nuclear-magnetism cavity, mix for existing liquid superconduction nuclear magnetic resonance spectrometer
A kind of problem of even and synchronous in-situ study, there is provided liquid nuclear-magnetism automatic in-situ response analysis test system.
Liquid nuclear-magnetism automatic in-situ response analysis test system, it is characterised in that including liquid superconduction nuclear magnetic resonance spectrometer,
Reaction in-situ unit in chamber, agitating unit and control unit are transmitted outside chamber；Reaction in-situ unit includes the reaction that is nested in the chamber
Device, be nested reactor locking cap and action separation rotor；The reactor that is nested is including quartz tubular reactor and positioned at tubulose
Internal layer mozzle in quartz reactor；The reactor locking cap that is nested includes the outer tube lock being enclosed within outside quartz tubular reactor
Only cap, one end be connected with outer tube locking cap the other end be connected with inner tube locking cap and be enclosed within the locking inner core on internal layer mozzle and
The pipeline locking cap that is nested being connected with inner tube locking cap；It is described action separation rotor include rotor body, action release bearing and
The locking bushing outside quartz tubular reactor is enclosed within, the rotor body is connected by acting release bearing with locking bushing；Institute
Stating transmission agitating unit outside chamber includes that pipeline is transmitted/stirred to the set embedded being connected with the pipeline locking cap that is nested, be nested pipeline
Separator and accurate program controlled syringe pump, pipeline is transmitted/stirred to the set embedded includes that the stirring pipeline being mutually nested and sample are passed
Defeated pipeline, the pipeline separator that is nested includes separator main body, locking cap, and one end of the separator main body passes through locking cap
Pipeline is transmitted/stirs with the set embedded to be connected, remaining two ends is respectively by locking cap and two accurate program controlled syringe pumps
Syringe is connected；Described control unit includes the computer being connected by special communication cable with accurate program controlled syringe pump.
The pipeline separator that is nested includes locking bushing pipe, and the set embedded that locking bushing pipe in separator main body will separate is passed
The diameter amplification of the transfer line in defeated/stirring pipeline, is passed to locking cap and locks and seal with separator main body.
The utility model has advantages below compared with prior art：
（1）Developed on the basis of original traditional liquid superconduction nuclear magnetic resonance spectrometer it is a set of can be in liquid superconduction core
The reaction in-situ of addition reaction mass, reaction system mixing and synchronous on-line monitoring record is realized in nuclear magnetic resonance spectrometer cavity simultaneously
Monitoring system.For the further investigation of chemical catalysis reaction mechanism provides effective information, while the reactant to build efficient stable
System's research provides new technical support.
（2）In-situ characterization chemical reaction course changes.In catalytic reaction process, the monitoring of reaction process, reaction are middle
The capture of body is probed into the mechanism reacted, condition optimizing, side reaction occurrence condition etc. are significant.By liquid nuclear-magnetism certainly
The change that reaction in-situ analysis of test system can be with on-line checking reactant and catalyst during the course of the reaction is moved, accurate prison is reached
Survey the purpose of reaction process.
（3）The influence of reaction temperature, atmosphere and stirring to reaction process.React temperature, atmosphere and the stirring condition for occurring
Highly important effect is played to research light-catalyzed reaction mechanism, but most of reaction monitoring at this stage is required for destruction former
Carry out reaction condition, thus can realize not destroying reaction condition by liquid nuclear-magnetism automatic in-situ response analysis test system
Under the premise of the purpose of in-situ characterization is carried out to course of reaction.
（4）The foundation of liquid nuclear-magnetism automatic in-situ response analysis test system will be provided for liquid superconduction nuclear magnetic resonance spectrometer
One new analysis and testing technology, realized in monitoring process it is unattended so that the in-situ characterization means of abundant chemical reaction, prison
Efficiency high is surveyed, data are accurate, with very strong application value.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
Fig. 2 is the structural representation of reaction in-situ unit in chamber described in the utility model.
Fig. 3 is the structural representation of the reactor that is nested described in the utility model.
Fig. 4 is the structural representation of action separation rotor described in the utility model.
Fig. 5 is the structural representation of the pipeline separator that is nested described in the utility model.
In figure：A- liquid superconduction nuclear magnetic resonance spectrometers；Reaction in-situ unit in B- chambers；C- transmits agitating unit outside chamber；D-
Control unit；1- quartz tubular reactors；2- internal layer mozzles；3- rotor bodies；4- acts release bearing；5- locking bushings；
6- is nested reactor；7- acts separation rotor；8- outer tube locking caps；9- locking inner cores；10- inner tube locking caps；11,12- is nested
Pipeline locking cap；13- set embedded transmit/stir pipeline；14- is nested pipeline separator；15- separator main bodies；16,18,19- locks
Only cap；17- locking bushing pipes；20,21- accurate program controlled syringe pumps；22- special communication cables.
Specific embodiment
As shown in Fig. 1,2,3,4,5, liquid nuclear-magnetism automatic in-situ response analysis test system, including liquid superconduction nuclear-magnetism is common
Shake spectrometer A, reaction in-situ unit B in chamber, outside chamber transmit agitating unit C and control unit D；Reaction in-situ unit includes set in chamber
Embedding reactor 6, be nested reactor locking cap and action separation rotor 7；The reactor 6 that is nested includes quartz tubular reactor 1 and position
In the internal layer mozzle 2 in quartz tubular reactor 1；The reactor locking cap that is nested includes being enclosed within outside quartz tubular reactor 1
Outer tube locking cap 8, one end other end that is connected with outer tube locking cap 8 is connected and is enclosed within internal layer mozzle 2 with inner tube locking cap 10
Locking inner core 9 and the pipeline locking cap 11,12 that is nested that is connected with inner tube locking cap 10；Action separation rotor 7 includes rotor sheet
Body 3, action release bearing 4 and the locking bushing 5 being enclosed within outside quartz tubular reactor 1, rotor body 3 is by acting release bearing
4 are connected with locking bushing 5；Agitating unit is transmitted outside chamber includes that the set embedded being connected with the pipeline locking cap 11,12 that is nested is transmitted/stirred
Pipeline 13, the pipeline separator that is nested 14 and accurate program controlled syringe pump 20,21 are mixed, pipeline 13 is transmitted/stirred to set embedded to be included mutually
The stirring pipeline and sample transfer pipeline being nested, the pipeline separator that is nested 14 include separator main body 15, locking cap 16,18,19,
One end of separator main body 15 is transmitted/is stirred pipeline 13 and is connected by locking cap with set embedded, and remaining two ends passes through locking respectively
Cap is connected with the syringe on two accurate program controlled syringe pumps 20,21；Control unit includes logical with accurate program controlled syringe pump 20,21
Cross the connected computer of special communication cable 22.
The pipeline separator that is nested 14 includes locking bushing pipe 17, and locking bushing pipe 17 is nested the separation in separator main body 15
The diameter amplification of the transfer line in pipeline 13 is transmitted/stirred to formula, is passed to locking cap 19 and is locked simultaneously with separator main body 15
Sealing.
When liquid nuclear-magnetism automatic in-situ response analysis test system works, reaction in-situ unit B is placed in liquid superconduction in chamber
Within nuclear magnetic resonance spectrometer A cavitys, serve as situ reactor and nuclear magnetic tube.Wherein be nested the quartz tubular reactor 1 of reactor 6
It is reaction vessel, built-in reaction raw materials, in-situ chemical reaction is completed herein；The Main Function of internal layer mozzle 2 is stirred for auxiliary
And sample-adding；The acting as of action separation rotor 7 serves as rotor, and holding is nested reactor 6 in liquid superconduction nuclear magnetic resonance spectrometer A chambers
Correct position within body；The rotor body 3 for acting separation rotor 7 rotates within liquid superconduction nuclear magnetic resonance spectrometer A cavitys
While, the reactor 6 that is nested being connected with action release bearing 4, locking bushing 5 is not rotated, so as to avoid set embedded from passing
Defeated/stirring pipeline 13 twists；The Main Function of outer tube locking cap 8, locking inner core 9 and inner tube locking cap 10 is nested for sealing
Reactor 6 is simultaneously relatively fixed quartz tubular reactor 1 and the position of internal layer mozzle 2；Reaction in-situ unit B is by being nested in chamber
Pipeline locking cap 11,12, set embedded are transmitted/are stirred pipeline 13 and be connected with the pipeline separator 14 that is nested.Set embedded transmission/stirring pipe
Line 13 is made up of the stirring pipeline and sample transfer pipeline being mutually nested, and Main Function is transmission reaction raw materials, mixes reactant
System.The Main Function of the pipeline separator that is nested 14 be by cover embedded transmit/stir pipeline 13 the pipeline that is nested be separated into transmission and
Two independent pipelines of stirring, are connected with two accurate program controlled syringe pumps 20,21 respectively；Two accurate program controlled syringe pumps 20,21
Main Function be under the programme-control of control unit D for being provided with special control software, to allow whole system to carry out sample introduction and stir
Mix work.Liquid superconduction nuclear magnetic resonance spectrometer A is timed monitoring simultaneously.
Claims (2)
1. liquid nuclear-magnetism automatic in-situ response analysis test system, it is characterised in that including liquid superconduction nuclear magnetic resonance spectrometer, chamber
Agitating unit and control unit are transmitted outside interior reaction in-situ unit, chamber；Reaction in-situ unit includes the reactor that is nested in the chamber
（6）, be nested reactor locking cap and action separation rotor（7）；The reactor that is nested（6）Including quartz tubular reactor（1）
With positioned at quartz tubular reactor（1）Interior internal layer mozzle（2）；The reactor locking cap that is nested includes being enclosed within quartz tubular
Reactor（1）Outer outer tube locking cap（8）, one end and outer tube locking cap（8）Be connected the other end and inner tube locking cap（10）It is connected
And it is enclosed within internal layer mozzle（2）On locking inner core（9）And with inner tube locking cap（10）The connected pipeline locking cap that is nested（11,
12）；The action separation rotor（7）Including rotor body（3）, action release bearing（4）Be enclosed within quartz tubular reactor（1）
Outer locking bushing（5）, the rotor body（3）By acting release bearing（4）With locking bushing（5）It is connected；Outside the chamber
Transmission agitating unit includes and the pipeline locking cap that is nested（11,12）Connected set embedded transmits/stir pipeline（13）, be nested
Pipeline separator（14）With accurate program controlled syringe pump（20,21）, it is described set embedded transmit/stir pipeline（13）Including being mutually nested
Stirring pipeline and sample transfer pipeline, the pipeline separator that is nested（14）Including separator main body（15）, locking cap（16,
18,19）, the separator main body（15）One end by locking cap and it is described set embedded transmit/stir pipeline（13）It is connected, its
Remaining two ends pass through locking cap and two accurate program controlled syringe pumps respectively（20,21）On syringe be connected；Described control unit bag
Include and accurate program controlled syringe pump（20,21）By special communication cable（22）Connected computer.
2. liquid nuclear-magnetism automatic in-situ response analysis test system as claimed in claim 1, it is characterised in that the pipe that is nested
Road separator（14）Including locking bushing pipe（17）, locking bushing pipe（17）Will be in separator main body（15）The set embedded of interior separation is passed
Defeated/stirring pipeline（13）In transfer line diameter amplification, be passed to locking cap（19）With separator main body（15）Locking
And seal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621368678.6U CN206292192U (en) | 2016-12-14 | 2016-12-14 | Liquid nuclear-magnetism automatic in-situ response analysis test system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621368678.6U CN206292192U (en) | 2016-12-14 | 2016-12-14 | Liquid nuclear-magnetism automatic in-situ response analysis test system |
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| CN206292192U true CN206292192U (en) | 2017-06-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108226207A (en) * | 2016-12-14 | 2018-06-29 | 中国科学院兰州化学物理研究所 | Liquid nuclear-magnetism automatic in-situ response analysis tests system |
| CN110609053A (en) * | 2018-06-15 | 2019-12-24 | 中国科学院大连化学物理研究所 | In-situ chemical reactor and system for combining in-situ chemical reactor with nuclear magnetic resonance |
| CN111257363A (en) * | 2020-03-18 | 2020-06-09 | 厦门大学 | Front end of in-situ separation detection nuclear magnetic resonance radio frequency probe and preparation method thereof |
-
2016
- 2016-12-14 CN CN201621368678.6U patent/CN206292192U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108226207A (en) * | 2016-12-14 | 2018-06-29 | 中国科学院兰州化学物理研究所 | Liquid nuclear-magnetism automatic in-situ response analysis tests system |
| CN108226207B (en) * | 2016-12-14 | 2024-03-29 | 中国科学院兰州化学物理研究所 | Liquid nuclear magnetism automatic in-situ reaction analysis test system |
| CN110609053A (en) * | 2018-06-15 | 2019-12-24 | 中国科学院大连化学物理研究所 | In-situ chemical reactor and system for combining in-situ chemical reactor with nuclear magnetic resonance |
| CN111257363A (en) * | 2020-03-18 | 2020-06-09 | 厦门大学 | Front end of in-situ separation detection nuclear magnetic resonance radio frequency probe and preparation method thereof |
| CN111257363B (en) * | 2020-03-18 | 2021-02-19 | 厦门大学 | Front end of in-situ separation detection nuclear magnetic resonance radio frequency probe and preparation method thereof |
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