CN108499499B - Temperature-controllable micro continuous flow tube reactor - Google Patents
Temperature-controllable micro continuous flow tube reactor Download PDFInfo
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- CN108499499B CN108499499B CN201810291365.2A CN201810291365A CN108499499B CN 108499499 B CN108499499 B CN 108499499B CN 201810291365 A CN201810291365 A CN 201810291365A CN 108499499 B CN108499499 B CN 108499499B
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 122
- 239000012495 reaction gas Substances 0.000 claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 claims description 40
- 239000010949 copper Substances 0.000 claims description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 39
- 238000007789 sealing Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 10
- 239000004809 Teflon Substances 0.000 claims 1
- 229920006362 Teflon® Polymers 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 29
- 230000009257 reactivity Effects 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 5
- 238000004949 mass spectrometry Methods 0.000 abstract description 4
- 238000004868 gas analysis Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 30
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005040 ion trap Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00822—Metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00891—Feeding or evacuation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00954—Measured properties
- B01J2219/00961—Temperature
Abstract
The invention relates to a temperature-controllable micro continuous flow tube reactor, which comprises a reaction tube, a reaction tube sleeve sleeved outside the reaction tube, a funnel arranged at one end of the reaction tube, and a temperature control device connected to the side of the funnel. Compared with the prior art, the invention has low cost, the length of the flow tube is only 50mm, the reaction gas can fully collide and react with cluster ions, the ionic current and the ionic signal intensity are enhanced, the effective temperature control of the flow tube reactor can be realized, the research on the cluster reactivity is simple and effective, and the invention can be used for detecting the atmospheric pollution or being used in the fields of trace gas analysis and the like together with mass spectrometry.
Description
Technical Field
The invention relates to a flow tube reactor, in particular to a temperature-controllable micro continuous flow tube reactor.
Background
The apparatus for gas-phase cluster reaction generally comprises three functional parts: cluster generating device, cluster reaction device and ion detecting device. With the development of the cluster chemistry field, cluster reaction devices (reaction collision cells, ion traps, selective ion flow tubes, multi-ion laminar flow reaction tubes and the like) provide abundant information for the research of the metal cluster reactivity. Especially in the past decades, advances in cluster chemistry have been dominated by advances in ion trap and flow tube reactor technology.
Conventional flow tubes are too long (typically about 1m) and cause problems of mainly 2 points:
firstly, metastable substances generated by the cluster generation device pass through a long flow pipe, and are likely to agglomerate or collide with reactants after the products are subjected to collision induction dissociation, so that false and wrong information is detected by the ion detection device;
secondly, because the flow tube is too long, the ion current of the product detected by the ion detection device is seriously attenuated, so that the signal of the detected product is very weak, and further research and analysis are influenced. Secondly, as the generation of different cluster ions is accompanied with the change of the temperature of the buffer gas, the uncertain factors of cluster reactivity increasing the temperature are further researched in the traditional flow tube, and the result is not accurate enough.
Therefore, the design of a simple temperature-controllable micro continuous flow tube reactor is crucial to the research of further broadening the cluster reactivity.
Disclosure of Invention
The object of the present invention is to overcome the above-mentioned drawbacks of the prior art by providing a temperature-controllable micro continuous flow tube reactor.
The purpose of the invention can be realized by the following technical scheme:
a temperature-controlled micro continuous flow tube reactor comprising:
a reaction tube is arranged in the reaction tube,
a reaction tube sleeve sleeved outside the reaction tube,
the funnel that sets up in reaction tube one end is effectual gas shunt, prevents effectively that buffer gas from influencing the sharp flight of cluster ion, reinforcing ion current.
And the temperature control device is connected to the side of the funnel.
The length of the reaction tube is 40-60 mm.
The other end in the reaction tube be equipped with copper mesh and reaction gas water conservancy diversion copper pipe, wherein the copper mesh setting is close to the open end of reaction tube, around the reaction tube inboard, makes buffer gas's temperature reach reaction temperature rapidly through the copper mesh, reaction gas water conservancy diversion copper pipe is equipped with two and separates certain distance between the copper mesh, sets up along the radial of reaction tube, can effectively make reaction gas and cluster ion carry out the collision reaction.
One side of the reaction tube sleeve close to the funnel is communicated with a reaction gas drainage copper tube, and different reaction gases can be selectively filled according to different application occasions.
An interlayer is formed between the reaction tube and the sleeve of the reaction tube and can be used for storing different reaction gases.
The sealing gasket is arranged in the interlayer, can be made of aluminum nitride ceramics, can conduct heat but not conduct electricity, effectively isolates the reaction tube sleeve from the reaction tube, and then strengthens the sealing degree between the reaction tube and the reaction tube sleeve.
The temperature control device is provided with a control disc.
The control disc on be equipped with thermocouple and heating plate, use the thermocouple to carry out real-time detection to reaction temperature, use the heating plate to adjust reaction temperature, control disc and funnel and reaction tube are all that the metal is made, so can heat conduction each other, the heating plate can be effectively to flow tube reactor accuse temperature.
The control disc is connected with a polytetrafluoroethylene screw, so that heat conduction and non-conduction can be realized, and the temperature control device is effectively isolated from the buffer gas cavity.
The reaction tube, the sealing gasket, the reaction tube sleeve, the funnel and the control disc are sequentially connected along the axial direction, and the reaction tube, the copper mesh, the flow guide tube, the reaction tube sleeve, the flow guide tube, the funnel and the control disc are all made of red copper metal, so that the reaction tube is not easy to oxidize and has good heat conductivity.
When the invention is used, when different cluster generating devices generate a large amount of gas-phase cluster ions, the cluster ions can be introduced into the flow tube by buffer gas (such as He), and the arrangement of the copper net at the tail end of the flow tube can effectively reduce the temperature of the buffer gas to the reaction temperature; reaction gas stores in the middle of the sleeve intermediate layer on the reaction tube, two copper pipes are with reaction gas continuous water conservancy diversion to reaction tube central authorities, later can carry out abundant continuous collision reaction with the cluster ion, self length has been shortened greatly to the flow tube through this patent design, ion signal intensity has been strengthened, and the temperature control device of reaction tube front end can adjust reaction temperature, realize the temperature when control cluster reaction, simultaneously can jointly use with the mass spectrum and be applied to fields such as detection atmosphere pollution or trace gas.
Compared with the prior art, the temperature of the buffer gas can be reduced to the temperature of the copper mesh, namely the reaction temperature, because the buffer gas passes through the copper mesh arranged at the tail end of the reaction tube; the copper guide pipe in the reaction tube continuously guides the reaction gas to the center of the reaction tube, so that the reaction gas and cluster ions can be subjected to full continuous collision reaction. The heating plate can heat the control disc in the temperature control device, the control disc can transfer heat to the funnel, the funnel transfers heat to the reaction tube again, the reaction temperature can be freely adjusted under the cooperation of the thermocouple for detecting the temperature, the temperature of the cluster during reaction is controlled, and the temperature control device has the following advantages:
1. the cost is low: the flow tube reactor is mainly made of red copper metal, so that the design is simple, and the cost of the device is greatly reduced.
2. And (3) effective temperature control: the reaction tube is provided with a copper net which can enable the temperature of the buffer gas to reach the reaction temperature quickly; the temperature controller can effectively adjust the temperature of the reaction tube, thereby controlling the temperature of the reaction.
3. The reaction tube is short in length: the length of the reaction tube is only 50mm, the added reaction gas can effectively collide with reactants, the ionic current is enhanced, and the detected signal intensity of the product is improved (large cluster signals with the size of about 1nm can be detected).
4. The overhaul is convenient: all parts can be flexibly assembled and disassembled.
5. The application range is wide: the method is suitable for the research of all gas clusters, and can be used for detecting atmospheric pollution or used in the fields of trace gas analysis and the like together with mass spectrometry.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic structural view of the present invention;
FIG. 3 is a schematic structural view of a control disk;
FIG. 4 is a mass spectrum of a large-size pure gold anion cluster prepared by the method of the invention and reacting with nitric oxide at a temperature of 120K.
In fig. 1: 1-buffer gas cavity, 2-cluster generating device, 3-temperature-controllable micro continuous flow tube reactor, and 4-buffer gas inlet.
In fig. 2: 11-temperature control device, 12-front end aluminum nitride ceramic sealing gasket, 13-reaction tube sleeve, 14-funnel, 15-reaction gas guide copper tube, 16-tail end aluminum nitride ceramic sealing gasket, 17-copper net, 18-reaction tube, 19-reaction gas guide copper tube.
FIG. 3: 21-thermocouple, 22-heating plate, 23-polytetrafluoroethylene screw hole and 24-control disk.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Examples
A temperature-controllable micro continuous flow tube reactor is structurally shown in figure 2 and mainly comprises a reaction tube 18, a reaction tube sleeve 13, a funnel 14, a temperature control device 11 and the like, wherein the length of the reaction tube 18 is only 50mm, added reaction gas can effectively collide with reactants to react, ion current is enhanced, and the detected signal intensity of products is improved (large cluster signals with the size of about 1nm can be detected). The reaction tube sleeve 13 is sleeved outside the reaction tube, and forms an interlayer with the reaction tube 18, and can be used for storing different reaction gases. The sealing gasket is arranged in the interlayer, the front-end aluminum nitride ceramic sealing gasket 12 and the tail-end aluminum nitride ceramic sealing gasket 16 which are used in the embodiment are respectively arranged at the front end and the rear end, the sealing gasket made of aluminum nitride ceramic can conduct heat but not conduct electricity, the reaction tube sleeve and the reaction tube are effectively isolated, and then the sealing degree between the reaction tube and the reaction tube sleeve is enhanced.
The funnel 14 is provided at an opening at the front end of the reaction tube 18, and is an effective gas diverter to effectively prevent the buffer gas from affecting the linear flight of the cluster ions, thereby enhancing the ion current, and is further connected with a temperature control device 11 at the opening. The temperature control device is provided with a control disc 24. The structure of the control disc 24 is as shown in fig. 3, a thermocouple 21 and a heating plate 22 are arranged on the disc, the reaction temperature can be detected in real time by using the thermocouple, the reaction temperature can be adjusted by using the heating plate, and the control disc, the funnel and the reaction tube are all made of metal, so that heat can be conducted mutually, and the heating plate can effectively control the temperature of the flow tube reactor. The control disc is connected with a polytetrafluoroethylene screw hole 23 for mounting a polytetrafluoroethylene screw, the screw made of the material can conduct heat and electricity, and the temperature control device is effectively isolated from the buffer gas cavity. One side of the reaction tube sleeve 13 close to the funnel 14 is communicated with a reaction gas drainage copper tube 19 which can be selectively filled with different reaction gases according to different application occasions.
The end of the reaction tube 18 is provided with a copper net 17 and a reaction gas guide copper tube 15, wherein the copper net 17 is arranged at the opening end close to the reaction tube and surrounds the inner side of the reaction tube, the temperature of the buffer gas is enabled to reach the reaction temperature rapidly through the copper net 17, the reaction gas guide copper tube 15 is provided with two copper nets which are spaced at a certain distance from each other and arranged along the radial direction of the reaction tube, and the reaction gas and cluster ions can be effectively enabled to carry out collision reaction.
The reaction tube, the sealing gasket, the reaction tube sleeve, the funnel and the control disc are sequentially connected along the axial direction, and the reaction tube, the copper mesh, the reaction gas guide copper tube, the reaction tube sleeve, the drainage tube, the funnel and the control disc are all made of red copper metal, so that the reaction tube, the sealing gasket, the reaction tube sleeve, the drainage tube, the funnel and the control disc are not easy to oxidize and have good heat conductivity.
When the temperature-controllable micro continuous flow tube reactor is used, the structure is shown in figure 1, buffer gas enters the buffer gas cavity 1 from the buffer gas inlet 4, and cluster ions generated by the cluster generating device 2 drift to the temperature-controllable micro continuous flow tube reactor 3 along with the buffer gas.
The buffer gas passes through the copper mesh 17 at the tail end of the reaction tube in the device of the micro continuous flow tube reactor 3, so that the temperature of the buffer gas can quickly reach the reaction temperature; the two heating sheets 22 on the temperature control device 11 can heat the control disc 11, the control disc 11 can transfer heat to the funnel 14, the funnel transfers heat to the reaction tube 18, and the temperature of the reaction tube can be effectively adjusted under the cooperation of the thermocouple 21 for detecting temperature, so that the reaction temperature of cluster ions and reaction gas can be controlled.
The invention utilizes the reaction gas guide copper tube 19 to store the reaction gas, then in the interlayer formed by the reaction tube sleeve 13 and the reaction tube 18, the aluminum nitride ceramic sealing gasket 12 at the front end and the aluminum nitride ceramic sealing gasket 16 at the tail end enhance the tightness of the interlayer, the stored reaction gas is subjected to sufficient collision reaction with cluster ions drifting to the center of the reaction tube through the reaction gas guide copper tube 15, and as the length of the reaction tube 18 is only 50mm, the added reaction gas can effectively perform collision reaction with reactants, so that the ion current is enhanced, and the detected product signal intensity is improved (large cluster signals with the size of about 1nm can be detected).
FIG. 4 is a mass spectrum of the reaction between large-size pure gold anionic clusters of about 1nm and nitric oxide at 120K. As shown in the upper mass spectrogram in FIG. 4, the method can obtain large-size cluster ions of about 1nm, and the ion signal intensity is very strong and is easy to detect by mass spectrometry. As shown in the lower mass spectrogram in fig. 4, according to the device, the reaction temperature is controlled to 120K, nitric oxide reaction gas is stored in an interlayer between the reaction tube and the reaction sleeve through the drainage copper tube, the drainage copper tube can guide the nitric oxide reaction gas to the center of the reaction tube and react with cluster ions, the signal intensity of a cluster ion product generated after the reaction is very strong and is very easy to detect by mass spectrometry, and thus, the mass spectrogram of the cluster ion reaction product is obtained, and can be used for researching the reactivity of large-size pure gold anion clusters with the concentration of 1nm and the nitric oxide at the temperature of 120K. By analogy, when different reaction gases are filled or different metal materials are replaced or different reaction temperatures are controlled, the blank of understanding of the reactivity of large-size ion clusters of about 1nm with small molecule gases at different reaction temperatures can be filled.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (8)
1. A temperature-controlled micro-scale continuous flow tube reactor for gas-phase cluster reactions, the reactor comprising:
the length of the reaction tube is 40-60 mm;
the reaction tube sleeve is sleeved outside the reaction tube, and the reaction gas is arranged in an interlayer between the reaction tube sleeve and the reaction tube;
the reaction device comprises a funnel arranged at one end of a reaction tube, a copper net and a reaction gas guide copper tube which are arranged at the other end of the reaction tube, wherein the reaction gas guide copper tube is communicated with an interlayer, and the copper net, the reaction gas guide copper tube and the funnel are sequentially arranged along the cluster ion flowing direction; and the number of the first and second groups,
and the temperature control device is connected to the side of the funnel.
2. The temperature-controllable micro continuous flow tube reactor as recited in claim 1 wherein a reaction gas guide copper tube is connected to a side of the reaction tube sleeve adjacent to the funnel.
3. A temperature-controlled micro continuous flow tube reactor as claimed in claim 1, wherein an interlayer is formed between the reaction tube and the reaction tube sleeve.
4. The temperature-controllable micro continuous flow tube reactor according to claim 3, wherein a sealing gasket is disposed in said sandwich.
5. A temperature-controlled micro continuous flow tube reactor as claimed in claim 1, wherein the temperature control means is provided with a control disk.
6. The temperature-controllable micro continuous flow tube reactor as recited in claim 5 wherein the control disk is provided with a thermocouple.
7. The temperature-controllable micro continuous flow tube reactor as claimed in claim 5, wherein the control disk is provided with a heating plate.
8. The temperature-controllable micro continuous flow tube reactor as recited in claim 5 wherein the control disk is attached with teflon screws.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810291365.2A CN108499499B (en) | 2018-04-03 | 2018-04-03 | Temperature-controllable micro continuous flow tube reactor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810291365.2A CN108499499B (en) | 2018-04-03 | 2018-04-03 | Temperature-controllable micro continuous flow tube reactor |
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| CN108499499B true CN108499499B (en) | 2020-11-27 |
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| CN110026144B (en) * | 2019-04-18 | 2020-06-16 | 中国科学院化学研究所 | Device and method for gas-phase ion catalysis molecular macro conversion |
| CN111733392A (en) * | 2020-07-01 | 2020-10-02 | 中国科学院化学研究所 | Gas-phase cluster reaction device, reaction system and method |
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