CN106289539A - A kind of method and apparatus for real-time monitoring chemical reaction process - Google Patents
A kind of method and apparatus for real-time monitoring chemical reaction process Download PDFInfo
- Publication number
- CN106289539A CN106289539A CN201610802873.3A CN201610802873A CN106289539A CN 106289539 A CN106289539 A CN 106289539A CN 201610802873 A CN201610802873 A CN 201610802873A CN 106289539 A CN106289539 A CN 106289539A
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- Prior art keywords
- chemical reaction
- copper conductor
- real
- oscillograph
- reaction process
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000012544 monitoring process Methods 0.000 title claims abstract description 25
- 239000010408 film Substances 0.000 claims abstract description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052802 copper Inorganic materials 0.000 claims abstract description 29
- 239000010949 copper Substances 0.000 claims abstract description 29
- 239000004020 conductor Substances 0.000 claims abstract description 28
- 238000005485 electric heating Methods 0.000 claims abstract description 21
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 17
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 17
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 17
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000010409 thin film Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000012528 membrane Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 6
- 230000005616 pyroelectricity Effects 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000001755 magnetron sputter deposition Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000001548 drop coating Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/02—Constructional details
- G01J5/03—Arrangements for indicating or recording specially adapted for radiation pyrometers
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
A kind of method and apparatus for real-time monitoring chemical reaction process, method is first respectively to prepare thin film electrode at electric heating film upper and lower surface, with conductive silver paste, copper conductor is fixed on lower films electrode, and draws positive and negative electrode by copper conductor, obtain flexible thermal and release temperature sensor；Then PDMS is dropped in flexible thermal and releases on temperature sensor, make flexible thermal release temperature sensor and surrounded by PDMS film completely, only expose copper conductor, be then heating and curing, obtain flexible detection device；Finally flexible detection device is attached to the outside of beaker, with copper conductor, oscillograph is accessed positive and negative electrode, by controlling reaction density and the stir speed (S.S.) of solution, waveform on oscillograph interface is different, and method is easy and simple to handle, quick, stable, and apparatus structure is simple, the process that reaction occurs can be monitored in real time, precision and resolution are high, and the suitability is wide, can be used for the monitoring of multiple chemical reaction process.
Description
Technical field
The invention belongs to Chemical Reaction Engineering field, be specifically related to a kind of method for real-time monitoring chemical reaction process
And device.
Background technology
In the chemical reaction process of materials synthesis and performance characterization, the process of observing response, severe degree and performance thereof
Quality, to analytical reactions process and control product kind have and important effect.A lot of chemical reactions is the most adjoint
Generation and the absorption of heat, different according to the concentration of reactant, produce and the heat that absorbs is the most different.Therefore, pass through
The heat that monitoring produces can effective analytical chemistry reaction process.Existing chemical reaction heat is by thermocouple and red mostly
Outer thermal imaging system is monitored, but the accuracy and precision of both modes cannot meet the most accurate chemical analysis, leads
Cause analysis result is not accurate enough, and monitoring device is relatively costly.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of anti-for monitoring chemistry in real time
The method and apparatus answering process, the method is easy and simple to handle, quick, stable, and apparatus structure is simple, can monitor reaction in real time and occur
Process, precision and resolution are high, and the suitability is wide, can be used for the monitoring of multiple chemical reaction process.
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind of method for real-time monitoring chemical reaction process, comprises the following steps:
1) respectively prepare thin film electrode 2 at electric heating film 1 upper and lower surface, with conductive silver paste, copper conductor 3 is fixed on
On lower films electrode 2, and draw positive and negative electrode by copper conductor 3, obtain flexible thermal and release temperature sensor；
2) PDMS is dropped in flexible thermal and release on temperature sensor, make flexible thermal release temperature sensor completely thin by PDMS
Film 4 surrounds, and only exposes copper conductor 3, is then heated to 65 DEG C, keeps 4 hours solidifying, obtains flexible detection device；
3) flexible detection device 5 is attached to the outside of beaker 7, with copper conductor 3, oscillograph 6 is accessed positive and negative electrode, work as burning
When not having solution 8 to react in cup 7, oscillograph 6 interface is not changed in, and illustrates do not have electric current to flow through；Preparation reaction in beaker 7
During solution 8, reaction, there is waveform in the interface of oscillograph 6, illustrates to create electric current, by controlling the reaction density of solution and stirring
Mixing speed, the waveform on oscillograph 6 interface is different, by the real-time monitoring chemical reaction process of oscillograph 6.
A kind of device for real-time monitoring chemical reaction process, for flexible detection device, including electric heating film 1,
Electric heating film 1 upper and lower surface respectively prepares thin film electrode 2, and membrane electrode 2 connects copper conductor 3, is drawn by copper conductor 3
Going out positive and negative electrode, electric heating film 1, membrane electrode 2 are surrounded by PDMS film 4, copper conductor 3 stretches out outside PDMS film 4,
PDMS film 4 is attached on chemical reaction container to be measured, and connecting between the copper conductor 3 of positive and negative electrode has oscillograph 6.
Described electric heating film 1 is flexible pyroelectricity material, including PVDF and PMN-PT.
The thickness of described electric heating film 1 is 30-500 μm.
Described membrane electrode 2 includes metal, polymer or Graphene.
The thickness of described membrane electrode 2 is 10-50nm.
Described electric heating film 1 upper and lower surface prepare the method for membrane electrode 2 include wet method transfer method, spin-coating method or
Magnetically controlled sputter method.
It is an advantage of the current invention that:
The present invention, based on pyroelectricity temperature sensor, uses electric heating film 1 thermal change of chemical reaction process to be turned
Being changed to the signal of telecommunication that can monitor in real time, pyroelectricity material is the crystalline material with spontaneous polarization properties, when the temperature is changed, from
Send out polarization to change, the Partial charge of surface adsorption can be discharged, thus realize the temperature transition of change is become electric energy, pass through
Electric heating film 1 can be simple and efficient observation reaction generating process.The method is easy and simple to handle, quick, stable, apparatus structure
Simply, can monitor the process that reaction occurs, precision and resolution height in real time, the suitability is wide, can be used for multiple chemical reaction mistake
The monitoring of journey.
Accompanying drawing explanation
Fig. 1 is to manufacture flexible thermal to release the flow chart of temperature sensor, and figure (a) is to prepare electric heating film two sides thin-film electro
The schematic diagram of pole；Figure (b) is the schematic diagram preparing copper conductor on membrane electrode；Figure (c) is the flexible detection dress after PDMS encapsulation
The schematic diagram put.
Fig. 2 is the schematic diagram of flexible detection device monitoring chemical reaction thermal discharge, and figure (a) is not have chemical reaction in beaker
Installation drawing；Figure (b) beaker has the installation drawing of chemical reaction.
Detailed description of the invention
Below by drawings and Examples, the inventive method is described further.
Embodiment 1
A kind of method for real-time monitoring chemical reaction process, comprises the following steps:
1) with reference to Fig. 1, thin film electrode 2 is respectively prepared, with leading at electric heating film 1 upper and lower surface by wet method transfer method
Copper conductor 3 is fixed on lower films electrode 2 by electricity silver slurry, and electric heating film 1 is the PVDF thin film of thickness 100 μm, thin-film electro
Pole 2 material is Graphene, and draws positive and negative electrode by copper conductor 3, obtains flexible thermal and releases temperature sensor；
2) use the mode of drop coating, the PDMS that mass fraction is 10% is dropped in flexible thermal and releases on temperature sensor, make
Flexible thermal is released temperature sensor and is surrounded by PDMS film 4 completely, only exposes copper conductor 3, is then heated to 65 DEG C, keeps 4
Solidification in individual hour, obtains flexible detection device；
3) with reference to Fig. 2, flexible detection device 5 is attached to the outside of beaker 7, with copper conductor 3, oscillograph 6 is accessed positive negative electricity
Pole, when not having solution 8 to react in beaker 7, oscillograph 6 interface is not changed in, and illustrates do not have electric current to flow through；Beaker 7 is joined
When making certain density solution 8, reaction, there is waveform in the interface of oscillograph 6, illustrates to create electric current, and the reactant of solution 8 is
Dilute H2SO4With Ca (OH)2, by controlling reaction density and the stir speed (S.S.) of solution, the waveform on oscillograph 6 interface is different, passes through
Analyzing the electric signal waveform on oscillograph 6 interface can monitoring chemical reaction process in real time.
Embodiment 2
A kind of method for real-time monitoring chemical reaction process, comprises the following steps:
1) with reference to Fig. 1, thin film electrode 2 is respectively prepared, with leading at electric heating film 1 upper and lower surface by wet method transfer method
Copper conductor 3 is fixed on lower films electrode 2 by electricity silver slurry, and electric heating film 1 is the PVDF thin film of thickness 200 μm, thin-film electro
Pole 2 material is Graphene, and draws positive and negative electrode by copper conductor 3, obtains flexible thermal and releases temperature sensor；
2) using the mode of drop coating, the flexible thermal that the PDMS that mass fraction is 10% drops in Fig. 1 (a) releases electro-temperature sensing
On device, make flexible thermal release temperature sensor and surrounded by PDMS film 4 completely, only expose copper conductor 3, be then heated to 65
DEG C, keep 4 hours solidification use, obtain flexible detection device；
3) with reference to Fig. 2, flexible detection device 5 is attached to the outside of beaker 7, with copper conductor 3, oscillograph 6 is accessed positive negative electricity
Pole, when not having solution 8 to react in beaker 7, oscillograph 6 interface is not changed in, and illustrates do not have electric current to flow through；Beaker 7 is joined
When making certain density solution 8, reaction, there is waveform in the interface of oscillograph 6, illustrates to create electric current, and the reactant of solution 8 is
Dilute H2SO4With Ca (OH)2, by controlling reaction density and the stir speed (S.S.) of solution, the waveform on oscillograph 6 interface is different, passes through
Analyzing the electric signal waveform on oscillograph 6 interface can monitoring chemical reaction process in real time.
Claims (7)
1. the method for real-time monitoring chemical reaction process, it is characterised in that comprise the following steps:
1) respectively prepare thin film electrode (2) at electric heating film (1) upper and lower surface, with conductive silver paste, copper conductor (3) is fixed
On lower films electrode (2), and draw positive and negative electrode by copper conductor (3), obtain flexible thermal and release temperature sensor；
2) PDMS is dropped in flexible thermal and release on temperature sensor, make flexible thermal release temperature sensor completely by PDMS film
(4) surround, only expose copper conductor (3), be then heated to 65 DEG C, keep 4 hours solidifying, obtain flexible detection device；
3) flexible detection device (5) is attached to the outside of beaker (7), with copper conductor (3), oscillograph (6) is accessed positive and negative electrode,
When not having solution (8) to react in beaker (7), oscillograph (6) interface is not changed in, and illustrates do not have electric current to flow through；In beaker (7)
During solution (8) that middle preparation is reacted, reaction, there is waveform, illustrates to create electric current in the interface of oscillograph (6), molten by controlling
The reaction density of liquid and stir speed (S.S.), the waveform on oscillograph (6) interface is different, anti-by oscillograph (6) monitoring chemistry in real time
Answer process.
2. for a device for real-time monitoring chemical reaction process, for flexible detection device, it is characterised in that: include pyroelectricity
Thin film (1), respectively prepares thin film electrode (2) at electric heating film (1) upper and lower surface, and the upper connection of membrane electrode (2) has copper to lead
Line (3), draws positive and negative electrode by copper conductor (3), electric heating film (1), membrane electrode (2) is surrounded by PDMS film (4)
Living, copper conductor (3) stretches out PDMS film (4) outward, and PDMS film (4) is attached on chemical reaction container to be measured, positive and negative electrode
Connect between copper conductor (3) and have oscillograph (6).
A kind of method for real-time monitoring chemical reaction process the most according to claim 1, it is characterised in that: described
Electric heating film (1) is flexible pyroelectricity material, including PVDF and PMN-PT.
A kind of method for real-time monitoring chemical reaction process the most according to claim 1, it is characterised in that: described
The thickness of electric heating film (1) is 30-500 μm.
A kind of method for real-time monitoring chemical reaction process the most according to claim 1, it is characterised in that: described
Membrane electrode (2) includes metal, polymer or Graphene.
A kind of method for real-time monitoring chemical reaction process the most according to claim 1, it is characterised in that: described
The thickness of membrane electrode (2) is 10-50nm.
A kind of method for real-time monitoring chemical reaction process the most according to claim 1, it is characterised in that: described
The method preparing membrane electrode (2) at electric heating film (1) upper and lower surface includes wet method transfer method, spin-coating method or magnetron sputtering side
Method.
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| CN201610802873.3A CN106289539A (en) | 2016-09-06 | 2016-09-06 | A kind of method and apparatus for real-time monitoring chemical reaction process |
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| CN201610802873.3A CN106289539A (en) | 2016-09-06 | 2016-09-06 | A kind of method and apparatus for real-time monitoring chemical reaction process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4516027A (en) * | 1982-01-29 | 1985-05-07 | Preh Elektrofeinmechanische Werke Jakob Preh Nachf. Gmbh & Co. | Infrared detector |
| JPS63182532A (en) * | 1987-01-23 | 1988-07-27 | Murata Mfg Co Ltd | Temperature sensor and temperature detector using the same |
| CN1444025A (en) * | 2002-03-08 | 2003-09-24 | 宝安康电子(北京)有限公司 | Temperature measuring method for biological, chemical and bio-chemical fields and its equipment |
| CN101043065A (en) * | 2006-03-21 | 2007-09-26 | 同济大学 | Pyroelectric infrared detector and used detecting member |
| CN101246055A (en) * | 2008-03-13 | 2008-08-20 | 电子科技大学 | Lithium tantalate thin film infrared detector and manufacturing method |
| CN101251422A (en) * | 2008-04-02 | 2008-08-27 | 中国科学院上海技术物理研究所 | Ultraviolet electricity scaling hot-dispelling electric detector |
| CN101881666A (en) * | 2009-05-08 | 2010-11-10 | 世纪晶源科技有限公司 | Film-type pyroelectric infrared sensor and preparation method thereof |
| CN102359821A (en) * | 2011-08-23 | 2012-02-22 | 郑州炜盛电子科技有限公司 | Pyroelectric infrared-sensitive element and pyroelectric infrared detector |
| CN103649719A (en) * | 2011-04-06 | 2014-03-19 | 维瓦克塔有限公司 | A device for detecting an analyte |
| CN105552206A (en) * | 2015-12-12 | 2016-05-04 | 西安交通大学 | Manufacturing method of flexible implantable power supply based on infrared light remote charging |
-
2016
- 2016-09-06 CN CN201610802873.3A patent/CN106289539A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4516027A (en) * | 1982-01-29 | 1985-05-07 | Preh Elektrofeinmechanische Werke Jakob Preh Nachf. Gmbh & Co. | Infrared detector |
| JPS63182532A (en) * | 1987-01-23 | 1988-07-27 | Murata Mfg Co Ltd | Temperature sensor and temperature detector using the same |
| CN1444025A (en) * | 2002-03-08 | 2003-09-24 | 宝安康电子(北京)有限公司 | Temperature measuring method for biological, chemical and bio-chemical fields and its equipment |
| CN101043065A (en) * | 2006-03-21 | 2007-09-26 | 同济大学 | Pyroelectric infrared detector and used detecting member |
| CN101246055A (en) * | 2008-03-13 | 2008-08-20 | 电子科技大学 | Lithium tantalate thin film infrared detector and manufacturing method |
| CN101251422A (en) * | 2008-04-02 | 2008-08-27 | 中国科学院上海技术物理研究所 | Ultraviolet electricity scaling hot-dispelling electric detector |
| CN101881666A (en) * | 2009-05-08 | 2010-11-10 | 世纪晶源科技有限公司 | Film-type pyroelectric infrared sensor and preparation method thereof |
| CN103649719A (en) * | 2011-04-06 | 2014-03-19 | 维瓦克塔有限公司 | A device for detecting an analyte |
| CN102359821A (en) * | 2011-08-23 | 2012-02-22 | 郑州炜盛电子科技有限公司 | Pyroelectric infrared-sensitive element and pyroelectric infrared detector |
| CN105552206A (en) * | 2015-12-12 | 2016-05-04 | 西安交通大学 | Manufacturing method of flexible implantable power supply based on infrared light remote charging |
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