CN206735816U - Percussion flow microwave heats coupled reaction device - Google Patents
Percussion flow microwave heats coupled reaction device Download PDFInfo
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- CN206735816U CN206735816U CN201621221380.2U CN201621221380U CN206735816U CN 206735816 U CN206735816 U CN 206735816U CN 201621221380 U CN201621221380 U CN 201621221380U CN 206735816 U CN206735816 U CN 206735816U
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- percussion flow
- inner bag
- microwave heating
- housing
- low pressure
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Abstract
Percussion flow microwave heats coupled reaction device, the utility model belongs to microwave attenuation materials reaction unit technical field, can solve to hit flow structure in the prior art does not have efficient percussion flow heater and the mixing of traditional agitating mode uneven, required incorporation time length, cause the problem of product quality is low, production efficiency declines.Including housing, microwave generator and percussion flow device, percussion flow device includes equal length and two feed tubes is arranged side by side, feed tube is respectively arranged below with opposite symmetrical two low pressure finer atomization nozzle, enclosure interior installs inner bag, two low pressure finer atomization nozzles are located in inner bag, temp measuring system is provided with inner bag, in the middle part of inner bag and bottom is equipped with sieve plate, bottom is picked out outside housing provided with discharging opening, housing side is equipped with cooler, reservoir is respectively equipped with the both sides less than percussion flow microwave heating coupled reactor, two reservoirs are connected with two feed tubes respectively.The utility model is simple in construction, and reactant quickly can be mixed and heated up simultaneously.
Description
Technical field
The utility model belongs to the technical field of microwave attenuation materials reaction unit, and specifically a kind of percussion flow-microwave adds
Thermal coupling reaction unit.
Background technology
Hydrothermal Synthesiss refer to that temperature is 100~1000 DEG C, pressure utilized in the aqueous solution under the conditions of being the GPa of 1 MPa~1
The carried out synthesis of material chemical reaction.Under subcritical and supercritical water heat condition, reaction is in molecular level, reactive
Raising allows hydro-thermal reaction to substitute some high temperature solid state reactions.Due to the homogeneous nucleation and nonhomogen-ous nucleation mechanism of hydro-thermal reaction
It is different from the flooding mechanism of solid phase reaction, thus noval chemical compound and new material that other methods can not be prepared can be createed.Mesh
Before be mainly used in the synthesis of crystal, ultra-fine grain, inorganic thin film, poromerics, in electronic material, magnetic material, optics material
The fields such as material, sensor material are also widely applied.
Percussion flow is to utilize two strands or a plurality of fluids fast ram, and strong turbulent-flow core heart district is formed between two feed pipes
Domain, the transmission of high momentum is carried out, tubulence energy dissipative shock wave is sharply increased, and because huge kinetic energy acts on, static pressure is switched at collision
Can, static energy effect makes its flow direction perpendicular to original direction, so as to produce strong microcosmic mixing.Determining Micromixing Characteristic Time and rapids
Kinetic energy dissipation rate is inversely proportional, i.e. tubulence energy dissipative shock wave is bigger, and Determining Micromixing Characteristic Time is smaller, and the effect of microcosmic mixing is better.It is microcosmic
The effect of mixing can directly affect the quality of product.Existing shock flow structure generally includes two feed tubes, is set on feed tube
There is nozzle, two nozzles are oppositely arranged：Feed tube is connected with nozzle in an angle of 90 degrees, and the liquid that two nozzles spray hits in opposite directions.Such as：
Chinese patent 201310338819.4, Chinese patent 200610102107.2 all disclose the shock flow structure of this form, but
Do not have efficient percussion flow heater at present.
Microwave is a kind of extremely short electromagnetic wave of wavelength, and the frequency range of microwave is 300MHz ~ 300KMHz, i.e., wavelength is in 1mm
~1000mm.Microwave heating is used exactly using microwave as a kind of energy, when microwave and material molecule interaction, production
Muon polarization estranged, orientation, friction, collision, absorb microwave energy and produce fuel factor.Microwave heating be object absorb microwave after itself
Heating, heats and is started simultaneously at from interior of articles, outside, can accomplish inside and outside while heat, and has and heats quick, uniform, operation side
Just the advantages that.At present, microwave attenuation materials technology is first to be mixed reactant through traditional agitating mode, is poured into after mixing poly-
Tetrafluoroethene reactor, is finally putting into microwave device and heats.Operating process is cumbersome discontinuous, and the mixing of traditional agitating mode is not
Uniformly, required incorporation time is longer, it will causes the problems such as product quality is low, production efficiency declines.
The content of the invention
The utility model aims to provide a kind of simple in construction, reactant while the Hydrothermal Synthesiss for quickly mixing and being rapidly heated
Reaction unit.While the mixing efficiency of present apparatus energy efficient hardening reactant realize be rapidly heated, have shorten the process time,
Make good product dispersibility, particle diameter distribution uniform, and run it is continuous, stably, low energy consumption the characteristics of.
The utility model adopts the following technical scheme that realization：
A kind of percussion flow-microwave heating coupled reaction device, including percussion flow-microwave heating coupled reactor, percussion flow-
Microwave heating coupled reactor includes housing, and case top is equipped with microwave generator and percussion flow device, and percussion flow device includes
Feed tube I and feed tube II, feed tube I and the equal length of feed tube II and it is arranged side by side, feed tube I and the lower section point of feed tube II
Not She You low pressure finer atomization nozzle I and low pressure finer atomization nozzle II, and low pressure finer atomization nozzle I and low pressure finer atomization
Nozzle II is symmetrical arranged in opposite directions, enclosure interior installation inner bag, and low pressure finer atomization nozzle I and low pressure finer atomization nozzle II are set
It is placed among inner bag, temp measuring system is provided with inner bag, the middle part and bottom of inner bag picks out shell equipped with sieve plate, bottom provided with discharging opening
Outside body, housing side is equipped with cooler, and reservoir is respectively equipped with the both sides less than percussion flow-microwave heating coupled reactor
A and reservoir B, reservoir A connect the feed tube I that percussion flow-microwave heats coupled reactor, liquid storage by pump I, flow meter I
Groove B connects the feed tube II that percussion flow-microwave heats coupled reactor by pump II, flow meter II.
Housing is the rectangle multimode casing of metallic walls closing, and housing is made of the material for being capable of microwave reflection, filled on housing
There are control panel and fire door.The microwave output power 1800W of microwave generator.Turn into multimode reflector under microwave radiation,
Internal liquid can be made quickly to heat.
Inner bag is that cylinder is nested in housing, and volume is about the 1/2-2/3 of housing, and inner bag is made of plastic material,
Inner bag is made of plastic material, and a segment distance is left between case top at the top of inner bag, is the high 1/10-1/5 of inner bag.
The middle part and bottom of inner bag are provided with good using polytetrafluoroethylene (PTFE) or other wetabilitys and suitable for microwave heating
Sieve plate made of material, the cm of a diameter of 0.8 cm ~ 1.2 sieve aperture is evenly distributed with the sieve plate, is ensureing intensity and use
While life-span, sieve plate is thin as far as possible, can so reduce difficulty of processing, increases rate of heat transfer, and reduce cost.The sieve plate face
Product is the 1/3 ~ 3/4 of interior plate, there is big surface area to become reconciled liquid wetting, is flowed to after liquid knockout on sieve plate,
Liquid meeting wetting and spreading film forming, increases boundary, reduces the speed of downward liquid flow, so as to extend the residence time, improves and passes
Matter efficiency, promote chemical reaction.
Cooler is connected with water inlet pipe I and outlet pipe II respectively, and water inlet pipe I is connected to regulating valve.Cooler can realize regulation
Cooling.
From the commercially available low pressure finer atomization nozzle that nozzle bore is the mm of 0.5 mm ~ 0.8, low pressure finer atomization nozzle I
（1.3）With low pressure finer atomization nozzle II（1.4）The distance betweenLForL=(0.6~4) d 0 , whereind 0 For nozzle bore.
Reservoir A and reservoir B is closed cell, avoids volatility of raw material, and blocking chemically reacts with air contact.Liquid storage
Groove A and reservoir B and feed tube I and the outer wall of feed tube II are equipped with heating and heat-insulating device.
Temp measuring system includes plating tetrafluoro platinum resistance temperature sensor, and plating tetrafluoro platinum resistance temperature sensor signal output part connects
Connect the signal input part of control panel.
Housing is made of carbon fibre composite, and inner bag is using polytetrafluoroethylmaterial material or other or other plastic material
It is made, microwave energy can be absorbed by microwave penetration and not, the heating and heat-insulating device is heating tape.
Compared with prior art, the utility model overcomes that current traditional agitating mode incorporation time is long, mixing efficiency is low
It is slow with heating, it is impossible to the shortcomings of adapting to the synthetic reaction demand such as molecular sieve, it is quick while there is liquid to be quickly well mixed
The advantages of heating, realize good microcosmic mixing；Meanwhile coupled with microwave heating, greatly improve Hydrothermal Synthesiss efficiency, especially
It is applied to the reaction system for preparing molecular sieve.
For traditional hydrothermal synthesis method prepares molecular sieve technique, first, the blend step of silicon source and silicon source need to lead to
Magnetic stirring apparatus completion is crossed, because magneton is local stirring, therefore, mixed effect is bad, less efficient, general mixing time
For 3h.Secondly, gained mixture, which need to be transferred in hydrothermal synthesis reaction kettle, carries out crystallization, length and made molecule the time required to crystallization
It is relevant to sieve species, digestion time, crystallization temperature, from a few houres to several days.And the utility model can make liquid-liquid in microcosmic ring
Realize that Quick uniform mixes under border, its incorporation time is only Microsecond grade, and this high-efficiency heating mode is carried out to it using microwave
Crystallization, the microwave crystallization time needed for different reactions are different.The utility model realization while quick mixing is rapidly heated,
Both continuously complete simultaneously, so as to highly shortened the reaction time.Raw material is more uniformly distributed through impact-flow equipment mixing, gained production
Thing particle diameter is smaller, evenly so as to improving product quality.In addition, apparatus structure described in the utility model is simple, small volume, easily
Operate, energy consumption is low and easy care.
Brief description of the drawings
Fig. 1 is percussion flow-microwave heating coupled reaction device technique flow chart；
Fig. 2 is percussion flow-microwave heating coupled reactor structural representation；
1 is that percussion flow-microwave heats coupled reactor in figure；2 be power supply；3 be flow meter I；4 be flow meter II；5 be valve
Door I；6 be valve II；7 be pump I；Pump II 8；9 be reservoir A；10 be reservoir B；
1.1 be feed tube I；1.2 be feed tube II；1.3 be low pressure finer atomization nozzle I；1.4 be that low pressure finer atomization is sprayed
Mouth II；1.5 be microwave generator；1.6 be control panel；1.7 be plating tetrafluoro platinum resistance temperature sensor；1.8 be sieve version；1.9
For discharging opening；1.10 it is inner bag；1.11 it is fire door；1.12 it is regulating valve；1.13 it is water inlet pipe；1.14 it is outlet pipe；1.15 it is
Housing.
Embodiment
The utility model is further illustrated below by embodiment, but is not limited to following examples.
Percussion flow-microwave heating coupled reaction device, including percussion flow-microwave heating coupled reactor 1, including housing
1.15 housings 1.15 are the rectangle multimode casing of metallic walls closing, and microwave generator 1.5 and percussion flow dress are installed in top respectively
Put, nozzle is low pressure finer atomization nozzle wherein used in percussion flow device, and middle part installs inner bag 1.10, is provided with and surveys in inner bag 1.10
Warm system（Temp measuring system can be optical fiber temperature-measurement, infrared measurement of temperature or platinum resistance thermometric）, temp measuring system preferably plates tetrafluoro platinum
RTD 1.7, sieve plate 1.8 is housed at the middle part of inner bag 1.10 and bottom, bottom is provided with discharging opening 1.9, housing
1.15 left sides are equipped with cooler, and cooler difference water inlet pipe I 1.13 is connected with outlet pipe II 1.14, and water inlet pipe I 1.13 is connected to tune
Valve 1.12 is saved, regulation cooling can be realized.Housing 1.15 is provided with control panel 1.6, controllable switch and temperature.Positioned at this dress
Put lower end both sides and be respectively equipped with reservoir A9 and reservoir B10, and percussion flow device is connected by pump, flowmeter respectively.It is tied
Structure and process chart are as shown in Figure 1.
Housing 1.15 with carbon fibre composite or other can the material of microwave reflection be made, turn into more under microwave radiation
Mould reflector, internal liquid can be made quickly to heat.
Inner bag 1.10 is that cylinder is nested in housing 1.15, and volume is about the 1/2-2/3 of housing 1.15, and inner bag is using modeling
Material material is made, and a segment distance is left between case top at the top of inner bag, is the high 1/10-1/5 of inner bag, housing 1.15 is using poly-
Tetrafluoroethene material or other plastic materials are made, and microwave energy can be absorbed by microwave penetration and not.
The middle part and bottom of housing 1.15 are equipped with sieve plate 1.8, and sieve diameter is the cm of 0.8 cm ~ 1.2, can increase material
Residence time and mass transfer rate.
Percussion flow device is installed on above the center of polytetrafluoroethylliner liner, including feed tube I 1.1 and feed tube II
1.2, feed pipe is made of stainless steel, can microwave reflection, liquid in pipe is not heated, and heated after liquid knockout.
Feed tube I 1.1 and the equal length of feed tube II 1.2 and it is arranged side by side.Feed liquor feed tube I 1.1 and feed tube II 1.2
The nozzle of lower end inside be low pressure finer atomization nozzle, and two nozzles are symmetrical arranged in opposite directions, injector spacing from forL=(0.6~4)d 0 。
Microwave generator 1.5 is made up of magnetron and matching component, and with temp measuring system in inner bag 1.10（Optical fiber temperature-measurement,
Infrared measurement of temperature, platinum resistance thermometric）It is connected, liquid heating and temperature control is at 100 ~ 180 DEG C.
Reservoir A9 and reservoir B10 passes through pump, the feed tube I 1.1 and feed tube II of flowmeter coupled reaction device respectively
1.2, reservoir is arranged to closed cell, avoids material liquid from being chemically reacted with air contact, in reservoir and feed liquor pipe outer wall
It is equipped with heating and heat-insulating device.The heating and heat-insulating device is heating tape.
Embodiment 1：Percussion flow-microwave heating coupled reaction device is applied to synthesis nano-ZSM-5 molecular sieve.
The percussion flow provided in the present embodiment-microwave heating coupled reaction device, including microwave generator 1.5, plating tetrafluoro
Platinum resistance temperature sensor 1.7, control panel 1.6 form temperature control system；Inner bag 1.10 is placed in inside housing 1.15, inner bag
1.15 it is polytetrafluoroethylmaterial material；Liquid distribution trough with tetraethyl orthosilicate, sodium hydroxide, crystal seed mixed solution inlet by being connected
Feed tube be connected with aluminum sulfate solution inlet feed tube composition；The bottom opening of housing 1.15 welds discharging opening 1.9, reaction
The molecular sieve suspension of synthesis is directly discharged from discharging opening 1.9.Two finer atomization injector spacings fromLFor 3mm.
Sodium hydroxide 8g, aluminum sulfate 1.1g, 4-propyl bromide 17.8g are taken, is dissolved with deionized water 504.3g, and add
2.8g crystal seeds, the silica gel of this silicon source mixed liquor and 133g containing crystal seed is added separately in reservoir A and B, by noncorrosive pump 7
With 8 with 20L/h input flow reactor, two strands of liquid are sprayed by nozzle 1.3 and 1.4, in polytetrafluoroethylliner liner 1.10
Impingement mix, realize quick, uniform microcosmic mixing, reaction.At the same time, it is 1800W to send power by microwave generator 1.5
Microwave in polytetrafluoroethylliner liner 1.10 liquid carry out microwave heating, heat 20mins after, finally from liquid outlet 1.8
Discharge, filtered, washing, dry, the ZSM-5 molecular sieve powder that granularity is 150 ~ 200nm is made after calcining.
Synthesis nano-ZSM-5 molecular sieve comprises the following steps that：
（1）Agitating device is opened, tetraethyl orthosilicate, sodium hydroxide, crystal seed mixed solution are configured in A reservoirs, it rubs
Your ratio is 4.4TPAOH:0.1Na2O:25SiO2:756H2O:100EtOH, the aluminum sulfate that 1.5mol/L is configured in B reservoirs are molten
Liquid；
（2）Noncorrosive pump is opened, is controlled the volume flow of two kinds of solution of A, B in 20L/h by adjusting flowmeter, will
Two kinds of material liquids are delivered to progress liquid liquid haptoreaction in reactor simultaneously, and fan-shaped liquid level is formed in contact surface；
（3）Open reactor, by adjustment control panel by the temperature adjustment of reactor be 180 DEG C, circular response 20
After minute, reactant is discharged from liquid outlet；
ZSM-5 molecular sieve powder is made in the ZSM-5 molecular sieve slurries of synthesis after filtering, wash, dry, calcine, and puts down
Equal particle diameter is 200nm.
Claims (9)
- A kind of 1. percussion flow-microwave heating coupled reaction device, it is characterised in that：Including percussion flow-microwave heating coupled reaction Device（1）, percussion flow-microwave heating coupled reactor（1）Including housing（1.15）, housing（1.15）Top is equipped with microwave generator （1.5）With percussion flow device, percussion flow device includes feed tube I（1.1）With feed tube II（1.2）, feed tube I（1.1）With enter Liquid pipe II（1.2）Equal length and it is arranged side by side, feed tube I（1.1）With feed tube II（1.2）It is fine to be respectively arranged below with low pressure Atomizer I（1.3）With low pressure finer atomization nozzle II（1.4）, and low pressure finer atomization nozzle I（1.3）With low pressure fine mist Change nozzle II（1.4）It is symmetrical arranged in opposite directions, housing（1.15）Inside installation inner bag（1.10）, and low pressure finer atomization nozzle I （1.3）With low pressure finer atomization nozzle II（1.4）It is arranged at inner bag（1.10）Among, inner bag（1.10）In be provided with temp measuring system, Inner bag（1.10）Middle part and bottom sieve plate is housed（1.8）, bottom be provided with discharging opening（1.9）Pick out housing（1.15）Outside, shell Body（1.15）Side is equipped with cooler, less than percussion flow-microwave heating coupled reactor（1）Both sides be respectively equipped with reservoir A（9）With reservoir B（10）, reservoir A（9）Pass through pump I（7）, flow meter I（3）Connect percussion flow-microwave heating coupled reaction Device（1）Feed tube I（1.1）, reservoir B（10）Pass through pump II（8）, flow meter II（4）Connect percussion flow-microwave heating coupling Reactor（1）Feed tube II（1.2）.
- 2. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that using being capable of microwave reflection Material made of housing（1.15）For the rectangle multimode casing of metallic walls closing, housing（1.15）It is upper that control panel is housed （1.6）And fire door（1.11）.
- 3. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that inner bag（1.10）For circle Cylindricality is nested in housing（1.15）Interior, volume is housing（1.15）1/2-2/3, inner bag（1.10）Top and housing（1.15）Top A segment distance is left between portion, is inner bag（1.10）High 1/10-1/5.
- 4. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that sieve plate（1.8）Area For inner bag（1.10）The 1/3 ~ 3/4 of bottom plate, sieve plate（1.8）On be evenly distributed with the cm of a diameter of 0.8 cm ~ 1.2 sieve aperture.
- 5. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that cooler is respectively with entering Water pipe I（1.13）With outlet pipe II（1.14）It is connected, water inlet pipe I（1.13）It is connected to regulating valve（1.12）.
- 6. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that low pressure finer atomization is sprayed Mouth is the mm of the mm of aperture 0.5 ~ 0.8 commercially available low pressure finer atomization nozzle, low pressure finer atomization nozzle I（1.3）It is fine with low pressure Atomizer II（1.4）The distance betweenLForL=(0.6~4) d 0 , whereind 0 For nozzle bore.
- 7. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that reservoir A（9）And storage Liquid bath B（10）For closed cell, reservoir A（9）With reservoir B（10）And feed tube I（1.1）With feed tube II（1.2）Outer wall It is equipped with heating and heat-insulating device.
- 8. percussion flow according to claim 1-microwave heating coupled reaction device, it is characterised in that temp measuring system includes plating Tetrafluoro platinum resistance temperature sensor（1.7）, plate tetrafluoro platinum resistance temperature sensor（1.7）Signal output part connects control panel （1.6）Signal input part.
- 9. percussion flow according to any one of claims 1 to 8-microwave heating coupled reaction device, it is characterised in that housing （1.15）It is made of carbon fibre composite, inner bag（1.10）It is made of polytetrafluoroethylmaterial material, the heating and thermal insulation dress It is heating tape to put.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621221380.2U CN206735816U (en) | 2016-11-14 | 2016-11-14 | Percussion flow microwave heats coupled reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621221380.2U CN206735816U (en) | 2016-11-14 | 2016-11-14 | Percussion flow microwave heats coupled reaction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206735816U true CN206735816U (en) | 2017-12-12 |
Family
ID=60555179
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621221380.2U Withdrawn - After Issue CN206735816U (en) | 2016-11-14 | 2016-11-14 | Percussion flow microwave heats coupled reaction device |
Country Status (1)
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| CN (1) | CN206735816U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395855A (en) * | 2016-11-14 | 2017-02-15 | 中北大学 | Impinging stream-microwave heating coupling reaction device |
| CN109126677A (en) * | 2018-10-24 | 2019-01-04 | 中国科学院高能物理研究所 | Reaction in-situ device |
| CN109833838A (en) * | 2019-03-13 | 2019-06-04 | 中北大学 | Percussion flow-ultraviolet catalytic coupling reaction device and application method |
-
2016
- 2016-11-14 CN CN201621221380.2U patent/CN206735816U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395855A (en) * | 2016-11-14 | 2017-02-15 | 中北大学 | Impinging stream-microwave heating coupling reaction device |
| CN106395855B (en) * | 2016-11-14 | 2018-06-26 | 中北大学 | Percussion flow-microwave heating coupled reaction device |
| CN109126677A (en) * | 2018-10-24 | 2019-01-04 | 中国科学院高能物理研究所 | Reaction in-situ device |
| CN109833838A (en) * | 2019-03-13 | 2019-06-04 | 中北大学 | Percussion flow-ultraviolet catalytic coupling reaction device and application method |
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Legal Events
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20171212 Effective date of abandoning: 20180626 |