CN208878550U - The continuous rapid microwave reaction system of constant temperature - Google Patents
The continuous rapid microwave reaction system of constant temperature Download PDFInfo
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- CN208878550U CN208878550U CN201821446744.6U CN201821446744U CN208878550U CN 208878550 U CN208878550 U CN 208878550U CN 201821446744 U CN201821446744 U CN 201821446744U CN 208878550 U CN208878550 U CN 208878550U
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Abstract
The utility model discloses a kind of continuous rapid microwave reaction system of constant temperature, including microwave generator, the set heart spiral pipe reactor being installed in microwave generator, material pusher, material pot, with the temperature and flow velocity coordinated control system of material pusher communication connection, the installing set heart spiral pipe reactor in microwave generator, the set heart spiral pipe reactor includes reactor body, at least one helix tube is installed in reactor body, helix tube is placed in heat transfer medium, temperature and flow velocity coordinated control system detection temperature and fluctuation, once temperature fluctuation is more than setting value, system is automatically stopped charging and enters product end to avoid unreacted material, guarantee the high level of homogeneity of product quality, so that reaction can carry out in constant temperature, effectively improve reaction effect, to improve product quality.Helix tube in reactor body can be one, and it is parallel in the same direction to be also possible to more helix tubes, guarantee that reaction mass flow direction is consistent, multitube can greatly improve production capacity parallel.
Description
Technical field
The utility model relates to a kind of microwave reaction systems, are to be related to one kind to can control product quality reality more specifically
The continuous rapid microwave reaction system of constant temperature that existing continuous high quality quickly produces.
Background technique
It is generally believed that the thermal effect of microwave is heated from selectivity of the microwave to polar compound: in polar molecule
Distribution of charges is uneven, and the energy of the rapid electromagnetic wave absorption of polar molecule energy, is acted on by molecular dipole with every in microwave field
Second 4.9x109 ultrahigh speed vibration, improves the average energy of molecule, mentions the reaction temperature in region sharply with speed
Height, to accelerate the progress of chemical reaction.In the past few decades, it is organic that microwave radiation promotes the research of chemical reaction to have become
A hot spot in chemical field.Compared with traditional reaction process, microwave radiation chemical reaction not only can significantly reduce
Reaction time is precisely controlled reaction temperature, and can also significantly improve reaction yield, improves product purity.Due to microwave technology
Have many advantages, such as that cleaning, efficient, energy consumption is low, pollution is few, thus in organic synthesis, chemical analysis, Environmental Chemistry and other chemistry
It is used widely in each branch field, has gradually formed microwave plasma analytical chemistry.Microwave sample dissolving, microwave abstracting,
Desorption, dry, hygrometric, microwave pre-concentration and purification etc. are also comparatively fast developed.The application of microwave is almost throughout each of chemistry
A branch field.
Microwave radiation promote chemical synthesis be divided into again it is intermittent with two kinds of continous way.It is anti-that intermittent reaction is also known as mass
It answers, is suitable for preparing on a small scale, it is not easy to realize large-scale continuous production, once production scale amplification or anti-using large size
Answer device, mass transfer and heat transfer problem are just more prominent, and product quality reduces, possessed by microwave radiation chemical reaction quickly heating and
Inward natures' advantages such as rapid cooling will be offset or even completely lose.Serialization microwave chemical reaction in recent years gradually at
For important Land use systems, in continuous reaction, reaction stream heated by microwave area is quickly complete under certain temperature and pressure
At reaction.Microwave continuous reaction in, the design of reaction system and reactor is extremely critical, be control product quality and at
Originally, the core of production efficiency is improved.
Utility model content
To overcome drawbacks described above in the prior art, the utility model provide it is a kind of can monitor reaction temperature in real time, make anti-
Temperature and material flow is answered to link, and the continuous rapid microwave reaction system of constant temperature for effectively improving the yield and quality of product.
To achieve the above object, the utility model provides a kind of continuous rapid microwave reaction system of constant temperature, including microwave hair
Raw device, set heart spiral pipe reactor, the material pusher, material pot being installed in microwave generator, with material pusher
The temperature and flow velocity coordinated control system of communication connection, the set heart spiral pipe reactor includes reactor body, is installed in and answers
The intrinsic at least one helix tube of device, the reactor body are provided with heat transfer medium, and helix tube is placed in heat transfer medium, institute
The feed inlet for stating helix tube is connect by feed pipe with material pusher, and the discharge port of the helix tube is connect with discharge nozzle,
Cooling exchanger is installed on the discharge nozzle, the temperature and flow velocity coordinated control system include being installed on reactor body
For detecting the temperature-detecting device of heat-transfer medium temperature, the letter of the temperature-detecting device and temperature and flow velocity coordinated control system
Number input terminal is connected, and the temperature and the signal output end of flow velocity coordinated control system are connected by communication with material pusher
It connects.
Preferably, being provided with electromagnetic agitation in the set heart helix tube reactor body and material pot.
Preferably, being also installed with the condensing reflux for preventing heat transfer medium gasification to be lost on the reactor body
It manages, condenser is installed in condensing reflux pipe, there is the condenser pipe gone out for cooling liquid stream to export for one end of the condenser, described
The other end of condenser has the condensation tube inlet entered for cooling liquid stream.
Preferably, there is the cooling exchanger gone out for cooling liquid stream to export for one end of the cooling exchanger, it is described
The other end of cooling exchanger has the cooling exchanger entrance entered for cooling liquid stream.
Preferably, the temperature of the heat transfer medium is 40 DEG C -700 DEG C.
Preferably, the helix tube is one, helix tube is horizontally set in reactor body, the center of helix tube
The center line of line and feed pipe is in the same horizontal line.
Preferably, the helix tube is at least two, the center line of each helix tube is parallel to each other and is located at same water
In plane, the center line of each helix tube and the center line of corresponding feed pipe are in the same horizontal line.
Preferably, the helix tube has the identical or different radius of spin.
Preferably, one end of the discharge nozzle is connected with the filter for being separated by solid-liquid separation to material.
Preferably, the heat transfer medium is that heating is oily, the wall of the helix tube and microwave generator is glass structure
Part or polyvinyl fluoride component.
Compared with prior art, the utility model has the beneficial effects that:
The utility model includes microwave generator, and set heart spiral pipe reactor, the material being installed in microwave generator push away
Device, material pot are sent, temperature and flow velocity linkage control system with material pusher communication connection are installed in microwave generator
Heart spiral pipe reactor is covered, the set heart spiral pipe reactor includes reactor body, installs at least one answering in device ontology
Helix tube, helix tube are placed in heat transfer medium, and temperature includes being installed on reactor body to be used for flow velocity coordinated control system
The temperature-detecting device of heat-transfer medium temperature is detected, which is connected with the signal input part of control system, institute
The signal output end for stating temperature and flow velocity coordinated control system is connected by communication with material pusher to be connect, temperature and flow velocity linkage control
System processed detects temperature and fluctuation by being inserted into the temperature-detecting device of heat transfer medium, once temperature fluctuation is more than setting value,
System is automatically stopped charging and enters product end to avoid unreacted material, guarantees the high level of homogeneity of product quality, so that instead
It should be able to be carried out in constant temperature, effectively improve reaction effect, to improve product quality.Helix tube in reactor body can be with
It is one, it is parallel in the same direction to be also possible to more helix tubes, guarantees that reaction mass flow direction is consistent, mostly parallel can be significantly with helix tube
Improve production capacity.The advantages that the utility model can make full use of the rapid reaction of microwave reaction and reduce energy consumption, while realizing production
The continuous of product quickly and large-scale production avoids the disadvantages of yield is few and noncontinuity of conventional intermittent microwave reaction,
And guarantee the high level of homogeneity of product quality.The utility model is applicable to the preparation of a variety of chemical reactions and multiple product.
Detailed description of the invention
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment
Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is this
Some embodiments of utility model, for those of ordinary skill in the art, without creative efforts, also
Other drawings may be obtained according to these drawings without any creative labor.
Fig. 1 is a kind of structure chart of the continuous rapid microwave reaction system of constant temperature provided by the embodiment of the utility model；
Fig. 2 is that a kind of continuous rapid microwave reaction system of constant temperature provided by the embodiment of the utility model has same-handed half
The structure chart of the set heart spiral pipe reactor of two spiral glass tubes of diameter；
Fig. 3 is that a kind of continuous rapid microwave reaction system of constant temperature provided by the embodiment of the utility model has different spirals half
The structure chart of the set heart spiral pipe reactor of two spiral glass tubes of diameter；
Fig. 4 is that a kind of platinum of the continuous rapid microwave reaction system preparation of constant temperature provided by the embodiment of the utility model is used to receive
State diagram of the rice grain under high power transmission electron microscope；
Fig. 5 is the statistical form to the partial size of the product Pt nanoparticle of Fig. 3.
Specific embodiment
It is practical new below in conjunction with this to keep the objectives, technical solutions, and advantages of the embodiments of the present invention clearer
Attached drawing in type embodiment, the technical scheme in the utility model embodiment is clearly and completely described, it is clear that is retouched
The embodiment stated is the utility model a part of the embodiment, instead of all the embodiments.Based on the implementation in the utility model
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The range of the utility model protection.
The embodiments of the present invention provide a kind of continuous rapid microwave reaction system of constant temperature.
Referring to FIG. 1, the utility model provides a kind of continuous rapid microwave reaction system of constant temperature, including microwave generator 5,
Set heart spiral pipe reactor 6, the material pusher 2, material pot 1 being installed in microwave generator 5, with material pusher 2
The temperature and flow velocity coordinated control system of communication connection, the set heart spiral pipe reactor 6 include reactor body 61, are installed in
At least one helix tube 10 in device ontology 61 is answered, the reactor body 61 is provided with heat transfer medium, and helix tube 10 is placed in biography
In thermal medium, the feed inlet of the helix tube 10 is connect by feed pipe 62 with material pusher 2, and the helix tube 10 goes out
Material mouth is connect with discharge nozzle 63, and cooling exchanger 7, the temperature and flow velocity coordinated control system are installed on the discharge nozzle 63
Including being installed on reactor body 61 for detecting the temperature-detecting device 9 of heat-transfer medium temperature, 9 He of temperature-detecting device
Temperature is connected with the signal input part of flow velocity coordinated control system, and the signal of the temperature and flow velocity coordinated control system exports
End is connected by communication with material pusher 2 to be connect.The temperature-detecting device 9 is thermocouple, and reaction mass is placed in material pot 1
Interior, when microwave generator 6 heats heat transfer medium, the thermocouple carries out thermometric to heat transfer medium, and measuring
Temperature signal is delivered in temperature and flow velocity coordinated control system via the signal input part of temperature and flow velocity coordinated control system,
When the temperature of heat transfer medium is between preset temperature, temperature and flow velocity coordinated control system issue signal to material and push
In device 2, material pusher 2 is acted, and the material in material pot 1 is directed into helix tube 10, when the temperature of heat transfer medium
When not between preset temperature, control system issues signal and send via conducting wire 3 into material pusher 2, material pusher 2
Stopping acts, and the material in material pot 1 stops entering in helix tube 10, realizes the thermostatic control to material reaction.It is described default
Temperature is 40 DEG C -700 DEG C, and the temperature of heat transfer medium is the temperature that material is reacted in helix tube 10, and heat transfer medium is deposited
It is being to guarantee that reaction carries out at a constant temperature in order to reduce temperature fluctuation and be precisely controlled temperature, improve product quality.The present embodiment
In, preferred heat-transfer medium temperature is 50 DEG C -450 DEG C, and heat transfer medium is preferably transparent heating oil, is preferably but not limited to silicon
Oil, in order to observe the reacting phenomenon in helix tube 10.
Electromagnetic agitation 11 is provided in the material pot 1, electromagnetic agitation 11 pairs of materials of son are stirred, so that material
Equalization of concentration reacts more stable.It is provided with electromagnetic agitation 11 in the heat transfer medium of the set heart helix tube reactor body 61,
Electromagnetic agitation 11 pairs of heat transfer mediums of son are stirred, so that the temperature equalization of heat transfer medium, to control the temperature of helix tube 10
It is balanced.
One end of the cooling exchanger 7 has the cooling exchanger outlet 71 gone out for cooling liquid stream, the cooling exchange
The other end of device 7 has the cooling exchanger entrance 72 entered for cooling liquid stream, will have been reacted in helix tube 10 using coolant liquid
Complete material carries out fast cooling when flowing out via discharge nozzle 63, and the material after cooling can be collected directly or by filter 12
It is being collected after being separated by solid-liquid separation.
It is installed with the condensing reflux pipe 41 for preventing heat transfer medium gasification to be lost on the reactor body 61, is condensed back to
Condenser 4 is installed in flow tube 41, one end of the condenser 4 has the condenser pipe outlet 15 gone out for cooling liquid stream, described cold
The other end of condenser 4 has the condensation tube inlet 14 entered for cooling liquid stream, is cooled back the heat transfer medium of gasification using coolant liquid
It flow in reactor body 61, prevents the loss of heat transfer medium, be further ensured that the equilibrium of reaction process temperature, improve product matter
Amount.
The helix tube 10 is placed horizontally in the heat transfer medium of the set heart spiral pipe reactor 6.
The reactor body 61 is provided with the opening 13 for heat transfer medium to be added.
Preferably, the temperature-detecting device 9 is thermocouple.
Referring to FIG. 1, the helix tube 10 is one, helix tube 10 is horizontally set in reactor body 61, helix tube
The center line of 10 center line and feed pipe 62 in the same horizontal line, guarantees feed flow rate accurate stable, improves material reaction
Quality.
Referring to FIG. 2, the helix tube 10 is two, misplaces between two helix tubes 10 and place, two helix tubes 10
Center line is parallel to each other and is located in same level, the center line of the center line of each helix tube 10 and corresponding feed pipe 62
In the same horizontal line, guarantee feed flow rate accurate stable, improve material reaction quality.Certainly, in other embodiments, described
Helix tube 10 may be three or more, misplaces and places between each helix tube 10, the center line of each helix tube 10 is parallel to each other simultaneously
In same level, the center line of each helix tube 10 and the center line of corresponding feed pipe 62 in the same horizontal line,
Guarantee feed flow rate accurate stable, improves material reaction quality.
Referring to FIG. 2, each helix tube 10 radius of spin having the same, referring to FIG. 3, each helix tube 10 is with different
The radius of spin.More helix tubes 10 are arranged can be improved the yield of unit time parallel, reduce energy consumption and production costs.
The material pusher 2 is peristaltic pump, the work of the temperature and flow velocity coordinated control system control peristaltic pump
State effectively controls reaction process to control the flow velocity that material flows into helix tube 10, improves product quality.
When reaction product is solidliquid mixture, one end of the discharge nozzle 63 is connected with for carrying out solid-liquid point to material
From filter 12, reaction while be separated by solid-liquid separation, the filter 12 be preferably but not limited to low pressure filter system.
The wall of the helix tube 10 and microwave generator 5 is glass component or polyvinyl fluoride component.
The selection of the heat transfer medium is based on temperature required for reacting, and reaction is not to be exceeded in General reactions temperature and pressure
The temperature and pressure that equipment matter can bear.The reaction temperature that the utility model can be born is room temperature to 700 degrees Celsius, preferably warm
Degree is 30 to 450 degrees Celsius.
The continuous rapid microwave reaction system of this constant temperature is suitable for homogeneous or heterogeneous phase chemical reaction, is especially suitable for preparation high price
The product of value, the noble metal catalyst of especially all kinds of support type high loadings, such as all kinds of single metal or alloys
Platinum base, palladium base, ruthenium-based catalyst.The quick preparation of high-value product, cooling and separation may be implemented in the reaction system, reduces energy
Consumption and operating cost.Realize the quick of the noble metal catalyst of all kinds of support type high loadings, continuously, large-scale production is suitble to
The preparation of for example high carrying capacity noble metal catalyst of high-value product, product quality homogeneity is good, applied widely.
Tool to carry out Pt nanoparticle manufacture using the continuous rapid microwave reaction system of constant temperature provided by the present application below
Body embodiment:
0.6 gram of homemade graphene dispersion is prepared into support dispersion into 60 milliliters of ethylene glycol, and is kept stirring spare.
1.08 grams of chloroplatinic acids are distributed in 100 milliliters of ethylene glycol and prepare metal precursor solutions, and 1.6 grams of citric acids are then added, sufficiently stir
After mixing half an hour, is mixed with support dispersion and continue 2 hours of high-speed stirred.With the ethylene glycol solution of sodium hydroxide, (1.0 rub
You/liter) pH value that adjusts mixture to 13, is further continued for stirring 2 hours, totally 170 milliliters of material total volume.Then constant temperature is started
Continuous rapid microwave reaction system sets reaction temperature as 150 degree by temperature and flow velocity coordinated control system, wriggling flow rate pump
For 10 ml/mins.When the temperature for covering the heat transfer medium in heart spiral pipe reactor reaches set temperature, peristaltic pump is open-minded,
Reaction mass starts the helix tube being sent in set heart spiral pipe reactor.Reaction time and subsequent push time have altogether 20 minutes.
1 gram of graphene-supported nm Pt catalyst that product is made after separation of solid and liquid, washing, freeze-drying, the mass content of platinum are
40%.Fig. 4 and Fig. 5 are please referred to, product is analyzed through high power transmission electron microscope (TEM) and the average grain through statistics discovery Pt nanoparticle
Diameter is 1.85 nanometers, and product is substantially better than similar commodity as the result is shown for this.
The continuous rapid microwave reaction system of this constant temperature is especially suitable for the product of preparation high value, and especially all kinds of support types are high
The noble metal catalyst of loading, such as platinum base, the palladium base, ruthenium-based catalyst of all kinds of single metal or alloys.The reaction
The quick preparation of high-value product, cooling and separation may be implemented in system, improves product quality, reduces energy consumption and production costs.
Above-described embodiment is the preferable embodiment of the utility model, but the embodiments of the present invention is not by above-mentioned
The limitation of embodiment, it is made under other any spiritual essence and principles without departing from the utility model to change, modify, replacing
In generation, simplifies combination, should be equivalent substitute mode, is included within the protection scope of the utility model.
Claims (10)
1. a kind of continuous rapid microwave reaction system of constant temperature, including microwave generator (5), it is characterised in that: further include being installed in
Set heart spiral pipe reactor (6), material pusher (2), material pot (1) in microwave generator (5), with material pusher
(2) temperature of communication connection and flow velocity coordinated control system, the set heart spiral pipe reactor (6) includes reactor body
(61), it is installed in at least one helix tube (10) answered in device ontology (61), the reactor body (61) is provided with heat transfer and is situated between
Matter, helix tube (10) are placed in heat transfer medium, and the feed inlet of the helix tube (10) is filled by feed pipe (62) and material push
(2) connection is set, the discharge port of the helix tube (10) is connect with discharge nozzle (63), is installed with cooling friendship on the discharge nozzle (63)
Parallel operation (7), the temperature and flow velocity coordinated control system include being installed on reactor body (61) for detecting heat transfer medium
The temperature-detecting device (9) of temperature, the signal input part phase of the temperature-detecting device (9) and temperature and flow velocity coordinated control system
The signal output end of connection, the temperature and flow velocity coordinated control system is connected by communication with material pusher (2) to be connect.
2. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the set heart helix tube is anti-
It answers and is provided with electromagnetic agitation (11) in device ontology (61) and material pot (1).
3. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the reactor body
(61) condensing reflux pipe (41) for preventing heat transfer medium gasification to be lost also is installed on, condensing reflux pipe is installed on (41)
There is the condenser pipe gone out for cooling liquid stream to export (15) for condenser (4), one end of the condenser (4), the condenser (4)
The other end has the condensation tube inlet (14) entered for cooling liquid stream.
4. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the cooling exchanger
(7) there is the cooling exchanger gone out for cooling liquid stream to export (71) for one end, and the other end of the cooling exchanger (7), which has, to be supplied
The cooling exchanger entrance (72) that coolant liquid flows into.
5. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the temperature of the heat transfer medium
Degree is 40 DEG C -700 DEG C.
6. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the helix tube (10) is
One, helix tube (10) is horizontally set in reactor body (61), in the center line of helix tube (10) and feed pipe (62)
Heart line is in the same horizontal line.
7. the continuous rapid microwave reaction system of constant temperature according to claim 1, it is characterised in that: the helix tube (10) is
At least two, the center line of each helix tube (10) is parallel to each other and is located in same level, the center line of each helix tube (10)
With the center line of corresponding feed pipe (62) in the same horizontal line.
8. the continuous rapid microwave reaction system of constant temperature according to claim 7, it is characterised in that: helix tube (10) tool
There is the identical or different radius of spin.
9. the continuous rapid microwave reaction system of constant temperature according to claim 1-8, it is characterised in that: the discharging
One end of pipe (63) is connected with the filter for being separated by solid-liquid separation to material.
10. the continuous rapid microwave reaction system of constant temperature according to claim 9, it is characterised in that: the heat transfer medium is
The wall of heating oil, the helix tube (10) and microwave generator (5) is glass component or polyvinyl fluoride component.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821446744.6U CN208878550U (en) | 2018-09-05 | 2018-09-05 | The continuous rapid microwave reaction system of constant temperature |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113083191A (en) * | 2021-03-31 | 2021-07-09 | 浙江锋源氢能科技有限公司 | Microwave reaction apparatus and control method thereof |
| WO2021188050A1 (en) * | 2020-03-17 | 2021-09-23 | Nanyang Technological University | Method for forming noble metal nanostructures on a support |
| CN114292629A (en) * | 2021-12-30 | 2022-04-08 | 北方民族大学 | Method for preparing phase change energy storage microcapsule by microwave and inorganic salt ultra-fast serialization and application thereof |
-
2018
- 2018-09-05 CN CN201821446744.6U patent/CN208878550U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021188050A1 (en) * | 2020-03-17 | 2021-09-23 | Nanyang Technological University | Method for forming noble metal nanostructures on a support |
| CN113083191A (en) * | 2021-03-31 | 2021-07-09 | 浙江锋源氢能科技有限公司 | Microwave reaction apparatus and control method thereof |
| CN114292629A (en) * | 2021-12-30 | 2022-04-08 | 北方民族大学 | Method for preparing phase change energy storage microcapsule by microwave and inorganic salt ultra-fast serialization and application thereof |
| CN114292629B (en) * | 2021-12-30 | 2024-01-30 | 北方民族大学 | Method for preparing phase-change energy-storage microcapsule by microwave synergistic inorganic salt ultra-fast continuous method and application thereof |
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