CN105080453B - Exocoel heating using microwave reactor, molecular sieve heating using microwave synthesis system and method in multi-source - Google Patents
Exocoel heating using microwave reactor, molecular sieve heating using microwave synthesis system and method in multi-source Download PDFInfo
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Abstract
The present invention discloses exocoel heating using microwave reactor, molecular sieve heating using microwave synthesis system and method in a kind of multi-source, this system can realize heating using microwave, be heated evenly, the industrial process of confined reaction, consecutive production, reach energy-conserving and environment-protective, the effect that crystallization is efficient, purity is high.The microwave reaction kettle uses many microwave sources, interior exocoel resonance structure to keep the advantage of resonator high field intensity.Multiple microwave source distribution energy regeneratives, pattern complementary can form relatively uniform pattern field distribution, be advantageously implemented the uniform heating of material in microwave reaction kettle.The airtight condition of production process is to replace keying by the electronic butterfly valve between feed hopper and heating using microwave kettle, heating using microwave kettle and insulation crystallization reaction kettle to realize simultaneously.Whole system uses the mode of production of " small kettle heating, big kettle insulation crystallization ", it is ensured that realize closed consecutive production.Equipment is designed using modular unit, is easy to by array combination, realizes improving the target of production capacity.
Description
Technical field
Invention is related to a kind of molecular sieve microwave compound probability production system and its heating using microwave kettle, and in particular to Yi Zhongduo
Exocoel molecular sieve heating using microwave reactor, molecular sieve consecutive production Microwave Synthesis System and method in source.
Background technology
Beta-zeolite molecular sieve be oil refining industry core catalyst material, it be with silicon-oxy tetrahedron and alumina on four sides
Body is basic structural unit, and the class that elementary cell is connected and composed is had cage type or duct by the oxygen bridge formed by oxygen atom
The silicon aluminate crystal of regular texture.It is in stones such as hydrogenation, cracking, isomerization, alkylation, alkene hydration, dewaxing and photocatalysis
Excellent catalytic performance is shown in numerous catalytic reactions of oil refining and petrochemical process.
At present, about 1,300,000,000 dollars of the annual sales amount of the main zeolite molecular sieve in Global Oil field, accounts for global catalyst
18.5%.Be present viscosity greatly in traditional class solid phase molecules sieve water-bath synthetic method, be heated uneven, and the crystallization process time is long, temperature
Degree is high, and energy consumption is big, the defect such as synthesis cost is high, hinders the popularization and application of the product.
The development of Pulse width technology is exactly to transform traditional industry technology in some aspects, improves device efficiency and produces
Moral character energy.Microwave class solid phase method technique is a kind of new technology, micro- compared with traditional beta-zeolite molecular sieve water-bath building-up process
Ripple class solid phase method is solvent-free, radiant body heating, and quick heating is selective to heating medium, makes many inorganic, organic reactions micro-
Under the conditions of wave radiation, can be completed with unconventional speed, turn brilliant rate high.In synthetic reaction process, material is under microwave field,
Polar molecule vibration at high speed, the severity of vibration is related to molecular dipole moment.Dipole moment is bigger, and the energy of electromagnetic wave absorption is healed
Rapidly, molecular activity is further acute, and the collision frequency of reactant molecule increases, while temperature rise is accelerated, causes the chance of synthetic reaction
Greatly enhance.And water-bath synthetic method, heat energy is that internal layer material is progressively sent into by top layer, and the time is long, uneven, energy consumption is big.Microwave
Method overcomes solid reunion and the uneven defect of particle that thermograde is caused, and initial stage a large amount of nucleation, induction period is short, obtains pure phase
And the suitable perfect cystal of size dimension, improve and turn brilliant speed.In closed container, temperature is raised other microwave action, instead
Answer the pressure of kettle to increase, promote and turn brilliant reaction.Compared with traditional water-bath synthetic method, microwave class solid phase method technique belongs to green
Chemical industry synthesis technology, it is with the obvious advantage.
After the experiment for carrying out microwave synthesis class solid phase beta-zeolite molecular sieve using microwave technology, preliminary test shows microwave
The method of method synthesis zeolite is superior to tradition at crystallization time, crystallization purity, turn brilliant aspect such as speed and microstructure
Water bath Method, such as turn brilliant time shorten to 10h or so from 60h, and temperature is down to 140 DEG C from 170 DEG C, and even lower, microwave method is produced
The sieve sample for going out is up to standard with standard comparison, crystallization purity after XRD is detected.But microwave current heating synthesis of molecular sieve
The research synthetic reaction experiments for being confined to micro-wave oven 100ml or so, Practical significance small more；Have no the medium-and-large-sized equipment of microwave for real
In the production of border.
The content of the invention
In view of this, the present invention provides exocoel heating using microwave reactor and molecular sieve heating using microwave in a kind of many microwave sources and closes
Into system, the closed continuity industrialized production to molecular sieve can be realized, and ensure to be heated evenly in reaction mass, molecular sieve
Crystallization purity is high.
Exocoel heating using microwave reactor includes in described multi-source：Inner chamber body, outer chamber and microwave source；The inner chamber body peace
Inside outer chamber, as material heating kettle；The outer chamber is metal material, and inner chamber body is the non-metallic material of wave transparent,
The inner chamber body is collectively forming microwave cavity with outer chamber；More than one waveguide feedback mouth is set in the cavity wall of outer chamber, is used
In connection microwave power source.
Ceramic seal window is provided with waveguide feedback mouth.Air inlet, air compression are provided with the outer chamber
Pump is inflated by air inlet to outer chamber.
Described molecular sieve heating using microwave synthesis system includes：Feed hopper, heating using microwave reactor, insulation crystallization reaction kettle
And microwave power source；The heating using microwave reactor includes the inner chamber body of non-metallic material and the outer chamber of metal material；Institute
State and set in the cavity wall of outer chamber more than one waveguide feedback mouth, for connecting microwave power source.
The integrated connection relation of the system is：The feed hopper is fixedly mounted on the top of heating using microwave reactor, charging
Valve is provided with passage between bucket and microwave reaction kettle；The bottom of the heating using microwave reactor is anti-with the insulation crystallization
The charging aperture of kettle is answered to be connected；The heating using microwave reactor bottom discharging opening and itself and insulation reaction kettle connecting portion between,
It is incubated crystallization reaction kettle its top feed mouthful and it is provided with valve and heating using microwave reactor connecting portion between.
Temperature for needed for maintaining crystallization process is constant, and heat-insulation layer is provided with the cavity wall of the insulation crystallization reaction kettle
And electric heat tracing device.
Used as a kind of preferred embodiment of the molecular sieve heating using microwave synthesis system, the molecular sieve heating using microwave synthesis system is entered
One step includes control unit and monitoring unit, and the monitoring unit includes being arranged on the heating using microwave reactor, insulation crystallization
Temperature sensor in reactor；The valve is electrically operated valve, and the feed hopper is automatic feed bucket, the motor-driven valve
Door, automatic feed bucket and microwave power source are controlled by described control unit.
As a kind of preferred embodiment of the molecular sieve heating using microwave synthesis system, the single molecular sieve heating using microwave is closed
Into system as a unit module, two or more unit module is controlled by a control unit.
As a kind of preferred embodiment of the molecular sieve heating using microwave synthesis system, in the heating using microwave reactor, exocoel
Internal portion sets two or more inner chamber body, and each inner chamber body has independent matched feed hopper and insulation crystallization reaction kettle.
Use the molecular sieve heating using microwave synthesis system carry out molecular sieve heating using microwave building-up process for：When initial, microwave
Valve, the valve of heating using microwave reactor discharge outlet and insulation crystallization reaction kettle charging aperture at heating response kettle charging aperture
The valve at place is in closed mode；
Step one：The valve that heating using microwave reactor charging aperture goes out is opened, the reaction chamber to heating using microwave reactor is built-in
Zeolite synthesis raw material is filled out, after the completion of filling, the valve that heating using microwave reactor charging aperture goes out is closed；It is micro- by microwave power source
Zeolite synthesis raw material in reaction chamber is heated to design temperature by ripple；
Step 2：Open the valve at the valve and insulation crystallization reaction kettle charging aperture of heating using microwave reactor discharge outlet
Door, makes the high temperature Zeolite synthesis raw material in reaction chamber after heating fall into insulation reaction kettle；
Step 3：After the Zeolite synthesis raw material in reaction chamber entirely falls in insulation crystallization reaction kettle, microwave is closed anti-
The valve at the valve and insulation reaction kettle charging aperture of kettle discharge outlet is answered, step one is back to；Until insulation crystallization reaction kettle
After high temperature Zeolite synthesis raw material after interior heating reaches setting capacity, insulation crystallization reaction kettle is changed.
Beneficial effect：
(1) using outer-cavity structure in multi-source, multiple microwave sources can realize that various modes are complementary and swear to heating using microwave reactor
Amount superposition, forms relatively uniform power distribution intensity, uniform field heating in heating using microwave reactor is advantageously implemented, so as to solve
Certainly inside reaction cavity being heated evenly property engineering problem；Outer-cavity structure ensure that multimode cavity power density is high in simultaneously
Advantage.
(2) whole heating using microwave synthetic molecules screen system is led to using the mode of production of " small kettle heating, big kettle insulation crystallization "
The valve crossed between feed hopper and heating using microwave kettle, heating using microwave kettle and insulation reaction kettle replaces keying, realizes closed continuity
Production, improve production efficiency, reducing energy consumption and pollution.
(3) many microwave source orthogonal optimizations are placed, the coherence that can reduce harmonic wave in microwave cavity, improve combined coefficient.
(4) system can realize volume production, to meet work as a unit module composition production array by centralized Control
The requirement that industry metaplasia is produced.
Brief description of the drawings
Fig. 1 is the structural representation of the zeolite molecular sieve Microwave Synthesis System in embodiment 1；
Fig. 2 is the top view of heating using microwave reactor in embodiment 2；
Fig. 3 is the top view of heating using microwave reactor in embodiment 3；
Fig. 4 is the structural representation that multiple zeolite molecular sieve Microwave Synthesis Systems form production array；
Fig. 5 is the schematic layout pattern that multiple heating using microwave reactors share outer chamber；
Fig. 6 is the functional block diagram of the molecular sieve heating using microwave synthesis system.
Wherein, 1- feed hoppers, 2- outer chambers, 3- inner chamber bodies, 4- waveguides feedback mouth, 5- electric press butterfly valve, 6- insulation crystallizations
Reactor, 7- air pressure pumps
Specific embodiment
Develop simultaneously embodiment below in conjunction with the accompanying drawings, and the present invention will be described in detail.
The present embodiment provides a kind of system for carrying out heating using microwave synthesis to beta-zeolite molecular sieve, using many microwave sources
Small heating kettle pattern is radiated, material thermally equivalent is advantageously implemented, the technique for meeting the continuous synthetically produced molecular sieve of microwave method will
Ask.
Embodiment 1：
The structure of the molecular sieve Microwave Synthesis System as shown in figure 1, including：Feed hopper 1, heating using microwave reactor, microwave
Power source, control unit, insulation crystallization reaction kettle 6 and multiple electric press butterfly valves 5.The feed hopper 1 is automatic feed bucket.
Wherein heating using microwave reactor is to complete the core that microwave energy intercouples with medium (Zeolite synthesis raw material)
Part, the heating using microwave reactor uses interior outer-cavity structure, and outer chamber 2 is hollow metal rectangular structure, and cavity wall material can
From the Stainless steel 316 L of addition (2~3%) Mo, the material has acid-alkali-corrosive-resisting performance, and atmospheric corrosion resistance and high temperature are strong
The characteristics of having spent, and cavity wall loss is smaller.The fixed inner chamber body 3 in the inside of outer chamber 2, the inner chamber body 3 is hollow ceramics circle
Cylinder, inner chamber body 3 uses electronic ceramics, and thermal losses is low, filling Zeolite synthesis raw material in inner chamber body 3.Outer chamber 2 and inner chamber body
3 are collectively forming microwave cavity, by the Zeolite synthesis raw material in the microwave power heating bore body 3 in microwave cavity.This kind is tied
The heating using microwave reactor power density of configuration formula is relatively high, and energy pressure-bearing, high temperature resistant etc.；Internal chamber wall energy loss is small, will be micro-
Wave energy efficient coupling is to material to be heated.
To make microwave field homogenize distribution, the purpose of uniform heating is realized, using multiport energy regenerative, four are set in Fig. 1
Microwave power source, thus is separately provided for connecting the waveguide of microwave power source on four sides in the metal rectangular chamber
Feedback mouth, feedback mouth uses standard waveguide, and four microwave sources are orthogonally located.During multiple microwave source forcings, using the position of its spatial distribution
Difference is put, implementation pattern is complementary, vector superposed, reach uniform heating purpose.To prevent microwave cavity inner waveguide from striking sparks, and to inner chamber
Body 3 plays reinforcement effect, ceramic seal window is set at waveguide feedback mouth, in order to fill compressed air in microwave cavity, in outer chamber 2
Upper setting air inlet and pressure ball valve, air pressure pump are inflated by air inlet pipe to microwave cavity.
The crystallization of the Zeolite synthesis raw material that the insulation crystallization reaction kettle is used for after heating, in the cavity wall of insulation reaction kettle
Heat-insulation layer and electric heat tracing device are provided with, it is constant with the temperature needed for the process for maintaining big kettle crystallization.
The integrated connection relation of the system is as shown in Figure 1：It is anti-that the feed hopper 1 is fixedly mounted on heating using microwave by bearing
Answer the top of kettle, for adding Zeolite synthesis raw material in heating using microwave reactor, feed hopper 1 and heating using microwave reactor it
Between passage be feeding-passage.Electric press butterfly valve is provided with feeding-passage, for opening or closing the feeding-passage
And play sealing function.The bottom of the heating using microwave reactor is connected by bearing with the charging aperture of insulation crystallization reaction kettle 6,
Passage between heating using microwave reactor and insulation crystallization reaction kettle 6 is tapping channel.In the heating using microwave reactor bottom
Discharging opening and itself and the connecting portion of insulation crystallization reaction kettle 6 between, its top feed mouthful of insulation crystallization reaction kettle 6 adds with itself and microwave
Electric press butterfly valve is provided between thermal response kettle connecting portion.Opened and closed by above three electric press butterfly valve, realized close
Close consecutive production.Above three electric press butterfly valve, feed hopper 1 and microwave power source are controlled by control unit, with reality
Now full-automatic continuous production.Connection between the heating using microwave reactor and insulation reaction kettle 6 simultaneously is automatic quick removable
Unload connection.
It is the convenience of description, makes the electric press butterfly valve on feeding-passage for valve A, heating using microwave reactor bottom discharging opening
Be valve B with itself and electric press butterfly valve between insulation reaction kettle connecting portion, insulation reaction kettle its top feed mouthful with itself and it is micro-
Electric press butterfly valve between Wave heating reactor connecting portion is valve C.When initial, valve A, valve B and valve C are turned off.The system
Functional module figure it is as shown in Figure 6.
After system sets electricity, control unit startup optimization sets related operational factor in control unit, and System self-test is complete
Bi Zhengchang, opens microwave source preheating.The power output of control unit Real-time Collection each microwave power source, reflection power, voltage,
Electric current, and can control the size of each microwave power source output.
Storage in Molecular sieve raw material storage device is transferred to after the completion of Zeolite synthesis raw material proportioning, when Molecular sieve raw material deposit
After the capacity of the Zeolite synthesis raw material in device reaches setting value, the signal that deposit is finished is sent to control unit；Control is single
Unit sends charging instruction after receiving the signal to self-feeding bucket, and opens valve A；The self-feeding bucket receives feed finger
After order, Zeolite synthesis raw material is filled to reaction chamber.After being filled to setting capacity, control unit shutoff valve A adjusts microwave work(
Class solid phase molecules in reaction chamber are sieved synthesis material and heated by the output in rate source by four microwave power sources.
Temperature sensor and pressure sensor are provided with the microwave cavity, in heating process, control unit Real-time Collection
And show the numerical value of temperature sensor and pressure sensor in reaction chamber.After the temperature in heating response chamber reaches setting value,
Control unit cuts off microwave power source, opens valve B and valve C, the class solid phase molecules after heating is sieved synthesis material and falls into insulation instead
Answer in kettle.Control unit opens passage blow device, it is ensured that the class solid phase molecules sieve synthesis material in passage is tried one's best and both falls within guarantor
In warm reactor, maintain passage clean.Purging finishes rear (purge time is set in control unit), control unit shutoff valve B
With valve C, valve A is opened, repeat to feed, heat, discharging process.Insulation crystallization reaction kettle is from after feeding in electric heat tracing device
Effect is lower to keep the constant of crystallization temperature, completes Crystallization of Zeolite process.
Due to the volume of the volume more than heating using microwave reactor of insulation reaction kettle, and crystallization process is more long, thus, can lead to
" small kettle heating, big kettle insulation crystallization " is crossed, continuous production is realized.After the raw material in insulation reaction kettle reaches its setting capacity,
On the premise of valve B and valve C is closed, control unit makes the connection between heating using microwave reactor and insulation crystallization reaction kettle automatically
Device is separated, and completes the replacing of insulation crystallization reaction kettle, and the work of heating using microwave reactor is not influenceed.
In system work process, airtight valve keying, temperature, pressure, voltage, electric current are different in control unit detects system
Chang Shi, cutting system power supply and automatic alarm, show corresponding fault-signal, are waited into system protection state and disposed.
Embodiment 2：
The structure type for being outer chamber 2 and inner chamber body 3 in heating using microwave reactor with the difference of above-described embodiment 1 is not
Together, the outer chamber 2 is the regular hexagon structure of hollow metal material, and inner chamber body 3 is hollow column construction, such as Fig. 2 institutes
Show, waveguide feedback mouth is respectively arranged with six sides of the outer chamber 2, for connecting microwave source.
Embodiment 3：
The structure type for being outer chamber 2 and inner chamber body 3 in heating using microwave reactor with the difference of above-described embodiment 1 is not
Together, the outer chamber 2 and inner chamber body 3 are hollow column construction, as shown in figure 3, the edge on the periphery of the outer chamber 2
Its circumference is evenly distributed with multiple waveguide feedback mouths, for connecting microwave source.
The outer chamber geometry body is not limited to rectangular cavities, polygon cavity, cylinder；Inner chamber body is not limited to cylinder
Body, cylinder bucking ladder structure.
Embodiment 4：
To meet the requirement of industrialized production, using above-mentioned heating using microwave synthesis system an as unit module, thus group
Into production array as shown in Figure 4, the unit module for constituting the production array is controlled by same control unit, is controlled by concentrating
System realizes volume production.
Embodiment 5：
Heating using microwave kettle is reacted using the heating using microwave of layout type as shown in Figure 5, i.e. two or more said system
Kettle shares an exocoel, and the outer chamber is internally provided with multiple inner chamber bodies.On the side wall of the outer chamber, needed according to bearing power
Microwave waveguide feedback mouth is set.Each inner chamber body has independent matched feed hopper and insulation crystallization reaction kettle, itself and charging
The annexation of bucket and insulation crystallization reaction kettle is same as described above.
The system is not limited to the synthesis of class solid phase molecules sieve, can also be applied to fluid microwave and uniformly heats, continuity life
The chemical field of product.
In sum, preferred application case study on implementation of the invention is these are only, the present invention can be applied in utilizing
The Application in Chemical Engineering similar field of heating using microwave reaction.It is above-mentioned to be not intended to limit the scope of the present invention, it is all of the invention
Within spirit and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (7)
1. molecular sieve heating using microwave synthesis system, it is characterised in that including：Feed hopper, heating using microwave reactor, insulation crystallization are anti-
Answer kettle and microwave power source；The heating using microwave reactor includes the inner chamber body of non-metallic material and the outer chamber of metal material；
Multiple waveguide feedback mouths are set in the cavity wall of the outer chamber, for connecting microwave power source, many microwave power source orthogonal optimizations
Place；The volume of the volume more than heating using microwave reactor of the insulation crystallization reaction kettle；
The integrated connection relation of the system is：The feed hopper is fixedly mounted on the top of heating using microwave reactor, feed hopper with
Passage between heating using microwave reactor is feeding-passage, and valve is provided with feeding-passage；The heating using microwave reactor
Bottom with it is described insulation crystallization reaction kettle charging aperture be connected, formation tapping channel；In the heating using microwave reactor bottom
Discharging opening and itself and insulation crystallization reaction kettle connecting portion between, insulation crystallization reaction kettle its top feed mouthful and itself and heating using microwave
Valve is provided between reactor connecting portion；
Zeolite synthesis raw material be class solid phase state, the molecular sieve heating using microwave synthesis system, further include control unit and
Monitoring unit, the monitoring unit includes the TEMP being arranged in the heating using microwave reactor, insulation crystallization reaction kettle
Device；The valve is electrically operated valve, and the feed hopper is automatic feed bucket, the electrically operated valve, automatic feed bucket and microwave
Power source is controlled by described control unit.
2. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that the chamber of the insulation crystallization reaction kettle
Heat-insulation layer and electric heat tracing device are provided with wall.
3. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that the heating using microwave reactor with protect
It is detachably connected between warm crystallization reaction kettle.
4. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that logical in the feeding-passage and discharging
Passage blow device is provided with road.
5. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that add the single molecular sieve microwave
Thermal synthesis system is controlled as a unit module, two or more unit module by a control unit.
6. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that in the heating using microwave reactor,
Outer chamber inside sets two or more inner chamber body, and each inner chamber body has independent matched feed hopper and insulation crystallization reaction
Kettle.
7. molecular sieve heating using microwave synthesis system as claimed in claim 1, it is characterised in that：The conjunction that molecular sieve heating using microwave is used
It is the mode of production of " small kettle heating, big kettle insulation crystallization " into method, when initial, the valve at heating using microwave reactor charging aperture
Valve at door, the valve of heating using microwave reactor discharge outlet and insulation crystallization reaction kettle charging aperture is in closing shape
State；The small kettle is heating using microwave reactor, and big kettle is insulation crystallization reaction kettle；
Step one：The valve that heating using microwave reactor charging aperture goes out is opened, to filling point in the reaction chamber of heating using microwave reactor
Son sieve synthesis material, after the completion of filling, closes the valve that heating using microwave reactor charging aperture goes out；Will by microwave power source microwave
Zeolite synthesis raw material in reaction chamber is heated to design temperature；
Step 2：The valve at the valve and insulation crystallization reaction kettle charging aperture of heating using microwave reactor discharge outlet is opened, is made
High temperature Zeolite synthesis raw material in reaction chamber after heating is fallen into insulation crystallization reaction kettle；
Step 3：After the Zeolite synthesis raw material in reaction chamber entirely falls in insulation crystallization reaction kettle, heating using microwave is closed anti-
The valve at the valve and insulation crystallization reaction kettle charging aperture of kettle discharge outlet is answered, step one is back to；Until insulation crystallization is anti-
After answering the high temperature Zeolite synthesis raw material in kettle after heating to reach setting capacity, insulation crystallization reaction kettle is changed.
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| CN201711147U (en) * | 2010-07-01 | 2011-01-19 | 张树槐 | High-power microwave tube-type continuous flow reactor |
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| CN103274428A (en) * | 2013-07-01 | 2013-09-04 | 中国海洋石油总公司 | Method of synthesizing nano Nu-10 molecular sieve by recycling mother solution |
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| MXPA06011294A (en) * | 2004-04-01 | 2007-01-16 | Dow Global Technologies Inc | Hydro-oxidation of hydrocarbons using catalyst prepared by microwave heating. |
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| CN201711147U (en) * | 2010-07-01 | 2011-01-19 | 张树槐 | High-power microwave tube-type continuous flow reactor |
| CN102855953A (en) * | 2012-04-27 | 2013-01-02 | 西南科技大学 | Continuous converting and sintering device for performing microwave high-temperature treatment on radioactive waste |
| CN102946655A (en) * | 2012-11-13 | 2013-02-27 | 中国石油大学(北京) | Microwave heating device capable of being continuously operated and resisting high temperature and high pressure and application thereof |
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