CN110652950B - Microwave coupling hypergravity reaction system for continuous production of porous materials - Google Patents
Microwave coupling hypergravity reaction system for continuous production of porous materials Download PDFInfo
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Abstract
The invention provides a microwave coupling hypergravity reaction system for continuous production of porous materials, which is characterized in that a hypergravity reactor, a microwave feeder, a first high-shear pump, a second high-shear pump and a filter are arranged, a hypergravity technology and a high-shear technology are combined, and the shearing force and the centrifugal force of the high-shear pump are utilized to ensure that materials meet the requirements of a homogenization process under the actions of high-speed shearing and frictional extrusion; by means of the characteristic of rapid micro-premixing of the hypergravity reactor, the nucleation process is carried out in a micro-uniform environment; the invention accurately controls the mass transfer rate and the heat transfer rate, and solves the problems of large production particles and uneven particle size distribution of the porous material caused by uneven mixing and uneven reaction temperature; the premixing stage and the crystallization stage are in the same reactor, so that the occupied area of equipment is saved, and the operation flow is simplified.
Description
Technical Field
The invention relates to the technical field of reactors, in particular to a microwave coupling hypergravity reaction system for continuous production of porous materials.
Background
At present, the synthesis of a large number of molecular sieves and porous materials is mainly carried out by a hydrothermal method or a solvothermal method, the synthesis of the molecular sieves and the porous materials by the two methods is almost divided into a premixing stage and a crystallization stage, and a large number of crystal nuclei are generated in the premixing stage, so that the number of the crystal nuclei can be increased by strengthening premixing, and the crystal nuclei are distributed in a system more uniformly; the crystallization stage needs to be performed in an environment with uniform concentration and temperature distribution, so that the structural units of the reaction system are uniformly distributed, and the particle size distribution of the final product can be uniform. Most of the currently proposed technologies have the problems of separation of a premixing stage and a crystallization stage, complex synthetic route, nonuniform mixing of slurry and a water phase or a solvent phase in a reaction system, incapability of continuous automatic production, and a plurality of defects.
Disclosure of Invention
In order to solve at least one of the above disadvantages, embodiments of the present application provide a microwave-coupled supergravity reaction system for continuous production of porous materials, including:
the system comprises a hypergravity reactor, a microwave feeder, a first high-shear pump, a second high-shear pump and a filter;
the first high shear pump forms a slurry by shearing reactants that produce the porous material;
the hypergravity reactor comprises a first cavity and a second cavity, wherein a rotating cavity is arranged in the first cavity and is used for premixing the slurry, and the premixed slurry is introduced into the second cavity to perform crystallization reaction;
the microwave feeder feeds microwaves into the first cavity and the second cavity;
the second high shear pump is used for shearing the unfinished product led out from the second cavity, and part of the unfinished product led out from the second cavity is led into the rotary cavity again, and part of the unfinished product led out from the second cavity is pumped into the filter;
the filter is used for separating the unfinished product and re-conveying the product which is not crystallized to the first high shear pump;
wherein, the product after crystallization separated by the filter is collected after washing and drying treatment.
In a preferred embodiment, valves are disposed on the pipeline between the filter and the second high shear pump and the pipeline between the high shear pump and the feed inlet of the supergravity reactor, and the microwave-coupled supergravity reaction system further comprises: a valve controller and a sample meter;
the sample meter is configured to measure a viscosity of the unfinished product introduced into the second high shear pump;
and the valve controller controls the switches of the two valves to reintroduce the unfinished product with the viscosity higher than the set threshold into the rotary chamber, and meanwhile, when the viscosity is lower than the set threshold, the valve controller introduces the unfinished product into the filter after a set time.
In a preferred embodiment, further comprising:
a cooler for cooling the unfinished product pumped to the filter by the second high shear pump.
In a preferred embodiment, the washing machine is a washing machine.
In a preferred embodiment, further comprising:
and the waste liquid treatment tank is used for collecting and treating the waste liquid separated by the cleaning machine.
In a preferred embodiment, further comprising:
and the dryer is used for drying the porous material cleaned by the cleaning machine.
In a preferred embodiment, the porous material is a molecular sieve.
In a preferred embodiment, the molecular sieve is: LTA type, FAU type, Y type, A type, MOR type, ZSM-5 type, beta type, AlPO type4One of series, SAPO series, TS-1 type, metal oxide molecular sieve, sulfide molecular sieve and metal organic compound molecular sieve.
In a preferred embodiment, a passive spoiler is disposed within the second cavity.
In a preferred embodiment, the passive spoiler comprises a plurality of blades.
The invention has the beneficial effects that:
the invention provides a microwave coupling hypergravity reaction system for continuous production of porous materials, which is characterized in that a hypergravity reactor, a microwave feeder, a first high-shear pump, a second high-shear pump and a filter are arranged, a hypergravity technology and a high-shear technology are combined, and the shearing force and the centrifugal force of the high-shear pump are utilized to ensure that materials meet the requirements of a homogenization process under the actions of high-speed shearing and frictional extrusion; by means of the characteristic of rapid micro-premixing of the hypergravity reactor, the nucleation process is carried out in a micro-uniform environment; the premixing and reaction temperature are accurately controlled by heating by means of a microwave technology, then the instruments are mutually matched to form a microwave coupling supergravity reaction system capable of realizing continuous production, and raw materials of the porous material sequentially pass through the instruments to form a product. In addition, the invention couples the supergravity technology and the microwave technology into the same reactor, and introduces the high shear pump technology to intensify mixing, which can accurately control the mass transfer and heat transfer rate, and solves the problems of large production particles and uneven particle size distribution of the porous material in industry caused by uneven mixing and uneven reaction temperature; meanwhile, the premixing stage and the crystallization stage are in the same reactor, so that the occupied area of equipment is saved, and the operation flow is simplified.
In a preferred technical scheme, the viscosity of the unfinished product of the second high shear pump is measured, so that the reaction stage of the unfinished product is judged according to the viscosity, the whole reaction system can be automatically switched to introduce the completely reacted product into a filter for collection through valve control, the unfinished product is reintroduced into the high gravity reactor for continuous mixing and crystallization reaction, the automatic production of the whole continuous production system is further realized, and the continuous production of the porous material is standardized.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows a schematic structural diagram of a microwave-coupled hypergravity reaction system for continuous production of porous materials in an embodiment of the invention.
FIG. 2 shows a schematic diagram of a hypergravity reactor in an embodiment of the invention.
FIG. 3a is a scanning electron microscope image of a ZSM-5 molecular sieve prepared by a conventional reaction vessel, FIG. 3b is a scanning electron microscope image of a ZSM-5 molecular sieve prepared in example 1 of the present invention, and FIG. 3c is a scanning electron microscope image of a commercial ZSM-5 molecular sieve.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Various cross-sectional views in accordance with the disclosed embodiment of the invention are shown in the drawings. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers, and relative sizes and positional relationships therebetween shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, as actually required.
Most of the currently proposed technologies have the problems of separation of a premixing stage and a crystallization stage, complex synthetic route, nonuniform mixing of slurry and a water phase or a solvent phase in a reaction system, incapability of continuous automatic production, and a plurality of defects.
Fig. 1 shows a microwave-coupled hypergravity reaction system for continuous production of porous materials in the embodiment of the application, and fig. 2 shows a specific structural schematic diagram of a hypergravity reactor, wherein the microwave-coupled hypergravity reaction system comprises: a high gravity reactor 3, a microwave feeder (not shown), a first high shear pump 21, a second high shear pump 22 and a filter 5; the first high shear pump 21 forms a slurry by shearing the reactants that produce the porous material; as shown in fig. 2, the high gravity reactor 33 includes a first cavity 31 and a second cavity 32, a rotating cavity 33 is disposed in the first cavity 31, the rotating cavity 33 is used for premixing the slurry, and the premixed slurry is introduced into the second cavity 32 to perform a crystallization reaction; the microwave feeder feeds microwaves into the first cavity 31 and the second cavity 32; the second high shear pump 22 is configured to shear the unfinished product discharged from the second cavity 32 and to reintroduce a portion of the unfinished product discharged through the second cavity 32 into the rotary chamber 33, and to pump a portion of the unfinished product discharged through the second cavity 32 into the filter 5; the filter 5 is used for product separation of the unfinished product and re-delivers the unfinished product to the first high shear pump 21; wherein, the product after crystallization separated by the filter 5 is collected after washing and drying treatment.
The method comprises the steps of setting a hypergravity reactor, a microwave feeder, a first high shear pump, a second high shear pump and a filter, combining a hypergravity technology and a high shear technology, and enabling the material to meet the homogenization process requirement under the action of high-speed shearing and frictional extrusion by means of the shearing force and the centrifugal force of the high shear pump; by means of the characteristic of rapid micro-premixing of the hypergravity reactor, the nucleation process is carried out in a micro-uniform environment; the premixing and reaction temperature are accurately controlled by heating by means of a microwave technology, then the instruments are mutually matched to form a microwave coupling supergravity reaction system capable of realizing continuous production, and raw materials of the porous material sequentially pass through the instruments to form a product. In addition, the invention couples the supergravity technology and the microwave technology into the same reactor, and introduces the high shear pump technology to intensify mixing, which can accurately control the mass transfer and heat transfer rate, and solves the problems of large production particles and uneven particle size distribution caused by uneven mixing and uneven reaction temperature of the molecular sieve and the porous material in industry; meanwhile, the premixing stage and the crystallization stage are in the same reactor, so that the occupied area of equipment is saved, and the operation flow is simplified.
In some embodiments, to facilitate continuous production, the reaction system of the present application further comprises a product feed tank 1 for introducing the slurry into a high gravity reactor 3.
It is understood that the porous material in the present application may be a carrier material having a pore structure, such as a molecular sieve, for example, the molecular sieve is: LTA type, FAU type, Y type, A type, MOR type, ZSM-5 type, beta type, AlPO type4One of series, SAPO series, TS-1 type, metal oxide molecular sieve, sulfide molecular sieve and metal organic compound molecular sieve.
Of course, other materials having a porous structure are possible, such as amorphous pore structure materials, including: silica gel, alumina gel, cross-linked clay, a layered column structure material and calcium phosphate; in addition, the material also comprises zeolite-like materials, mesoporous materials such as silicon oxide and the like, and macroporous materials, which are not limited and restricted by the application.
In some embodiments, please refer to fig. 2, a supergravity reactor in a microwave coupling supergravity reaction system includes a housing 35 having a receiving cavity, the receiving cavity is divided into a first cavity 31 located above and a second cavity 32 located below, a rotating cavity 33 is disposed in the first cavity 31, a rotating shaft 36 is fixed in a housing corresponding to the first cavity 31, the rotating cavity 33 includes a filler 37 and a housing 38 surrounding the rotating cavity of the filler, the housing 38 of the rotating cavity is fixedly connected to the rotating shaft 36 and further can be driven by the rotating shaft to rotate, a central portion of the filler 37 is a hollow structure, the hollow structure is inserted into a liquid distributor, a liquid or a fluid mixed with solid and liquid can be sprayed onto the filler through the liquid distributor 39, the rotating filler can cut the liquid or the fluid mixed with solid and liquid, and form micro-nano-scale micro elements in the first cavity 31, thereby achieving the sufficient premixing effect.
And the micro-nano-scale infinitesimal enters the second cavity under the action of gravity, and crystallization reaction nucleation is carried out to generate the porous material.
With continued reference to fig. 2, the microwave feeder comprises a plurality of probes 9 (for example, 4 probes shown in fig. 2), which are electrically connected to an external microwave generator (not shown) and function to feed microwaves into the first cavity 31 and the second cavity 32, wherein the microwaves have a heating effect and can uniformly heat the first cavity 31 and the second cavity 32.
In a preferred embodiment of the present application, a valve is disposed on a pipeline between the filter and the second high shear pump, and a pipeline between the high shear pump and the feed inlet of the supergravity reactor, and the microwave coupling supergravity reaction system further includes: a valve controller and a sample meter; the sample meter is configured to measure a viscosity of the unfinished product introduced into the second high shear pump; and the valve controller controls the switches of the two valves to reintroduce the unfinished product with the viscosity higher than the set threshold into the rotary chamber, and meanwhile, when the viscosity is lower than the set threshold, the valve controller introduces the unfinished product into the filter after a set time. In this example, experiments show that the viscosity of the premixed reactant is reduced continuously because the raw material is hydrolyzed continuously in the solution during the premixing process to generate a large number of structural units, the structural units exist stably in the initial gel, the viscosity of the raw material is high, and after the temperature is increased, the structural units are recombined continuously to form crystal nuclei, and finally, crystals are grown. After the structural units in the reaction feed liquid form crystals, the crystals exist in the feed liquid in the form of small solid particles, namely in the reaction process, the structural units are continuously reduced in the reaction feed liquid, so that the viscosity of the reaction feed liquid is continuously reduced, and when the viscosity reaches a certain fixed value, the reaction is completely carried out in a crystallization stage. Although the structural unit recombination still exists in the crystallization stage, the viscosity of the reaction feed liquid is not changed greatly.
In the preferred embodiment, since the reaction can be determined to be in the crystallization stage when the viscosity of the whole system is within a certain fixed value, when the detected viscosity is within a certain fixed value, the crystallization reaction has already started, and the crystallization reaction is completely completed after the longest crystallization time (from the beginning of crystallization to the end of crystallization), so that the crystallization reaction is inevitably completed as long as the set time is longer than or equal to the longest crystallization time, and the unfinished product is the product of the porous material.
The rotating chamber of the microwave coupling hypergravity reaction system is driven by a motor connected with a rotating shaft, and the invention does not limit the type and the variety of the motor.
For some special reaction needs, the microwave coupling hypergravity reaction system can be improved in structure, for example, in order to deal with a high-pressure system, an oil seal structure is added on the basis of the application; in order to deal with a heating system, a heat-insulating ring, a heating belt and the like are added on the basis of the application. The above modifications are all modifications that can be deduced by a person skilled in the art and the present invention is not exhaustive.
It should be noted that the micro-nano scale in the embodiments of the present application should be understood as a micro-nano scale or a nano-nano scale, that is, all the micro-nano scales in 1nm to 100 um.
In some embodiments, the filler material is nickel, copper, stainless steel, etc., for example, the filler material is stainless steel mesh, copper foam, ceramic foam. Material of fillerThe material can also be cordierite, sepiolite, foamed ceramic, foamed nickel or Al2O3The invention is not limited.
In some embodiments, the rotational speed of the microwave coupled hypergravity reaction system is 400rpm, 800rpm, 1200rpm, 1600rpm, 2000rpm, 2400rpm, which is not limited herein.
In some embodiments, the filler may be an integral filler, and the surface of the filler is subjected to the same treatment process, such as hydrophilic or hydrophobic treatment, and is adaptively adjusted according to a specific reaction system, which is not described herein again.
In one embodiment, the filler comprises a plurality of cut layers formed by a reel, and the first portion and the second portion each comprise at least one of the cut layers.
In one embodiment, two side surfaces of each cutting layer are respectively attached to one side surface of the adjacent cutting layer.
In some embodiments, the filler may be hydrophilically or hydrophobically treated to form a hydrophilic or hydrophobic surface.
The hydrophilic surface can be prepared by a sand blasting method, taking a stainless wire mesh as an example, the sand blasting method is to throw out quartz sand, carborundum, iron sand and the like by using compressed air as power, impact the surface of a workpiece at a high speed, and increase the rough structure of the surface of the stainless wire mesh by polishing, thereby obtaining the hydrophilic surface.
The hydrophobic surface is prepared by a multi-spray drying method. Taking a stainless steel wire mesh as an example, firstly adhering polytetrafluoroethylene powder on the surface of a common stainless steel wire mesh by using an electrostatic spraying method, and then placing the common stainless steel wire mesh adhered with the polytetrafluoroethylene powder in an oven at the temperature of 300-350 ℃ for about 30 minutes, wherein the process can remove a binder, a dispersing agent and a surfactant, so as to form a coated stainless steel wire mesh with a low surface energy material, namely a hydrophobic stainless steel wire mesh.
In some embodiments, the system further comprises: a cooler 4 for cooling the unfinished product pumped to the filter by the second high shear pump.
In addition, in some embodiments, the system further includes: a washing machine 7 for washing the crystallized product separated by the filter. The washing machine may be a centrifugal washing machine or the like.
Further, the above system further comprises: and a waste liquid treatment tank 10 for collecting and treating the waste liquid separated by the cleaning machine.
And, further comprising: and the dryer 8 is used for drying the porous material cleaned by the cleaning machine, and the product dried by the dryer 8 enters a product warehouse 11 for storage.
In some embodiments, the product directed through the filter 5 is transported by a first transport pump 61 and a second transport pump 62.
It will be appreciated that the hypergravity reactor of the present application is an external circulation vertical hypergravity rotating packed bed, but the same is true for vertical stators and rotors, for example, external circulation.
In some embodiments, the internal temperature of the external circulation hypergravity reactor is from 25 to 500 ℃.
The rotating speed of the external circulation hypergravity reactor is 500-2850 rpm.
The high shear pump throughput is 5-60m3The rpm was 4000 rpm.
The reaction material is introduced into an external circulation hypergravity reactor, circulated for a period of time and then heated by microwave. By adjusting the microwave feed power of the first cavity and the second cavity respectively, a reaction system with a temperature gradient can be formed, and certain specific reactions can be dealt with.
Preferably, the second cavity is internally provided with a passive turbulence member, so that the mixing in the crystallization reaction process is enhanced, the crystallization efficiency is accelerated, the concentration of reactants is uniform during crystallization, and the particle size difference of the generated product is small.
The passive spoiler may include a plurality of blades, which may be in a vertical state, an inclined state, or a horizontal state.
In addition, the junction of the first cavity and the second cavity can be provided with a dynamic seal.
When the premixing device is used, a reaction raw material is enabled to be homogeneous through the first high shear pump, then the homogeneous phase is sent into the rotary cavity through the liquid inlet, and the homogeneous phase is dispersed again through cutting of the filler to form micro elements with micro-nano scale, so that the premixing process is completed. Then the infinitesimal flow is in the second cavity under the action of gravity, further crystallization reaction is carried out, the passive turbulence member rotates in the second cavity to drive crystallized reactants to be uniformly mixed, crystallized unfinished products are pumped into the first cavity or the filter again through the second high-shear pump, depending on whether the final products are, the viscosity of the sample is measured through the sample meter, further the flow direction of the unfinished products passing through the high-shear pump can be automatically controlled, the purpose of automatically controlling continuous production is achieved, and crystallized products are collected through the filter, the cleaning machine, the dryer and the like to form porous materials.
Some specific scenario cases are given below to enhance understanding of the inventive concept of the present application.
Scenario case 1
Dissolving a certain amount of silica sol, aluminum sulfate, tetrapropylammonium hydroxide and a small amount of sodium chloride in deionized water, controlling the flow rate by using a flow meter, introducing the mixed feed liquid into an external circulation hypergravity reactor through a high-shear pump, repeatedly circulating the feed liquid for 30min through the high-shear pump, adjusting the microwave heating temperature to 130 ℃ for hydrothermal reaction, cooling the feed liquid through a cooler after 12h of reaction, introducing the cooled feed liquid into a falling film filter, washing until the pH is neutral, conveying the feed liquid to an HR series centrifuge through a screw pump after filtering, conveying the product to a micro-thermal regeneration compressed air dryer after centrifuging, and finally conveying the ZSM-5 molecular sieve to a product warehouse.
Scenario case 2
Taking a certain amount of H3PO4The method comprises the following steps of taking aluminum isopropoxide, silica sol, dipentamine and HCl solution as raw materials, controlling the flow rate through a flow meter, introducing the mixed feed liquid into an external circulation hypergravity reactor through a high shear pump, premixing for 10min, adjusting the microwave heating temperature to 175 ℃ for hydrothermal reaction, cooling, filtering, washing, centrifuging and drying the feed liquid after 10h of reaction to finally obtain the SAPO-31 molecular sieve.
Scenario case 3
Taking a certain amount of H3PO4Aluminum isopropoxide, triethylamine, HF solution (40% aqueous solution) and a small amount of C3H7OH is used as a raw material, flow is controlled through a flow meter, mixed feed liquid is introduced into an external circulation super-gravity reactor through a high shear pump, premixing is carried out at room temperature for 20min, the microwave heating temperature is adjusted to 180 ℃ for hydrothermal reaction, and after the reaction is carried out for 6h, the feed liquid is cooled, filtered, washed, centrifuged and dried to finally obtain the AlPO4-5 molecular sieve.
Scenario case 4
Adding GeO into water under hydrothermal system240% aqueous HF, ethylenediamine and small amounts of pyridine, ethylene glycol or butanol; and adding a small amount of water in a solvothermal system, wherein the mainly applied organic solvent comprises pyridine, ethylene glycol, ethanolamine, propanolamine, n-butanol, DMF (dimethyl formamide) and ethanol, introducing the mixed feed liquid into an external circulation hypergravity reactor through a high shear pump, premixing at room temperature for 30min, adjusting the microwave heating temperature to 180 ℃ for hydrothermal reaction, and cooling, filtering, washing, centrifuging and drying the feed liquid after 48h of reaction to finally obtain the germanate microporous compound.
Scene case 5
Dissolving a certain amount of di-n-butyl phosphate/1-butyl phosphoric acid/tri-n-butyl phosphorus oxide/tributyl phosphine, calcium chloride/calcium nitrate, ammonia water, ethyl orthosilicate and a template agent in deionized water, introducing the mixed feed liquid into an external circulation super-gravity reactor through a high-shear pump, premixing and reacting for 4 hours at room temperature, adjusting the microwave heating temperature to 100 ℃ for hydrolysis reaction, reacting for 12 hours, and cooling, filtering, washing, centrifuging and drying the feed liquid after the reaction to finally obtain the sodium phosphosilicate calcium nanospheres.
Dissolving a certain amount of silica sol/ethyl orthosilicate, titanium tetrachloride, ethylamine, water and tetrapropylammonium bromide/tetrapropylammonium chloride/tetrapropylammonium hydroxide in deionized water, introducing the mixed feed liquid into an external circulation hypergravity reactor through a high shear pump, premixing for 1h at room temperature, adjusting the microwave heating temperature to 170 ℃ for crystallization time of 48h, and cooling, filtering, washing, centrifuging and drying the crystallized feed liquid to finally obtain the small-grain TS-1 molecular sieve.
FIG. 3a is a scanning electron microscope image of a ZSM-5 molecular sieve prepared by using a conventional reaction vessel, FIG. 3b is a scanning electron microscope image of a ZSM-5 molecular sieve prepared in scenario case 1 of the embodiment of the present invention, and FIG. 3c is a scanning electron microscope image of a commercial ZSM-5 molecular sieve. It can be seen that the particle size distribution of fig. 3b is narrower, the morphology is uniform, the particle size is approximately circular, the average particle size is small, and the diffusion in the pores can be greatly reduced during use.
Obviously, through the detailed description of the above specific embodiments and the scenario cases, the present application combines the supergravity reactor, the microwave feeder, the first high shear pump, the second high shear pump and the filter, and combines the supergravity technology and the high shear technology, and with the aid of the shear force and the centrifugal force of the high shear pump, the material meets the homogenization process requirement under the action of high-speed shearing and frictional extrusion; by means of the characteristic of rapid micro-premixing of the hypergravity reactor, the nucleation process is carried out in a micro-uniform environment; the premixing and reaction temperature are accurately controlled by heating by means of a microwave technology, then the instruments are mutually matched to form a microwave coupling supergravity reaction system capable of realizing continuous production, and raw materials of the porous material sequentially pass through the instruments to form a product. In addition, the invention couples the supergravity technology and the microwave technology into the same reactor, and introduces the high shear pump technology to intensify mixing, which can accurately control the mass transfer and heat transfer rate, and solves the problems of large production particles and uneven particle size distribution caused by uneven mixing and uneven reaction temperature of the molecular sieve and the porous material in industry; meanwhile, the premixing stage and the crystallization stage are in the same reactor, so that the occupied area of equipment is saved, and the operation flow is simplified.
In a preferred technical scheme, the viscosity of the unfinished product of the second high shear pump is measured, so that the reaction stage of the unfinished product is judged according to the viscosity, the whole reaction system can be automatically switched to introduce the completely reacted product into a filter for collection through valve control, the unfinished product is reintroduced into the high gravity reactor for continuous mixing and crystallization reaction, the automatic production of the whole continuous production system is further realized, and the continuous production of the porous material is standardized.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (9)
1. A microwave coupling hypergravity reaction system for continuous production of porous materials is characterized by comprising:
the system comprises a hypergravity reactor, a microwave feeder, a first high-shear pump, a second high-shear pump and a filter;
the first high shear pump forms a slurry by shearing reactants that produce the porous material;
the hypergravity reactor comprises a first cavity and a second cavity, wherein a rotating cavity is arranged in the first cavity and is used for premixing the slurry, and the premixed slurry is introduced into the second cavity to perform crystallization reaction;
the microwave feeder feeds microwaves into the first cavity and the second cavity;
the second high shear pump is used for shearing the unfinished product led out from the second cavity, and part of the unfinished product led out from the second cavity is led into the rotary cavity again, and part of the unfinished product led out from the second cavity is pumped into the filter;
the filter is used for separating the unfinished product and re-conveying the product which is not crystallized to the first high shear pump;
wherein, the product after crystallization separated by the filter is collected after washing and drying treatment;
the filter with on the pipeline between the second high shear pump, and first high shear pump with be provided with the valve on the pipeline between the feed inlet of hypergravity reactor, microwave coupling hypergravity reaction system still includes: a valve controller and a sample meter;
the sample meter is configured to measure a viscosity of the unfinished product introduced into the second high shear pump;
and the valve controller controls the switches of the two valves to reintroduce the unfinished product with the viscosity higher than the set threshold value into the rotary chamber, and meanwhile, when the viscosity is lower than the set threshold value, the valve controller introduces the unfinished product into the filter after the set time.
2. The microwave-coupled hypergravity reaction system of claim 1, further comprising:
a cooler for cooling the unfinished product pumped to the filter by the second high shear pump.
3. The microwave-coupled hypergravity reaction system of claim 1, further comprising:
and the cleaning machine is used for washing the crystallized product separated by the filter.
4. The microwave-coupled hypergravity reaction system of claim 3, further comprising:
and the waste liquid treatment tank is used for collecting and treating the waste liquid separated by the cleaning machine.
5. The microwave-coupled hypergravity reaction system of claim 3, further comprising:
and the dryer is used for drying the porous material cleaned by the cleaning machine.
6. The microwave-coupled hypergravity reaction system of claim 1, wherein the porous material is a molecular sieve.
7. Root of herbaceous plantThe microwave-coupled hypergravity reaction system of claim 6, wherein the molecular sieve is: LTA type, FAU type, Y type, A type, MOR type, ZSM-5 type, beta type, AlPO type4One of series, SAPO series, TS-1 type, metal oxide molecular sieve, sulfide molecular sieve and metal organic compound molecular sieve.
8. The microwave-coupled hypergravity reaction system of claim 1, wherein a passive spoiler is disposed within the second cavity.
9. The microwave-coupled hypergravity reaction system of claim 8, wherein the passive spoiler comprises a plurality of blades.
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| CN110652950B (en) * | 2019-09-04 | 2021-04-23 | 北京化工大学 | Microwave coupling hypergravity reaction system for continuous production of porous materials |
| CN114804137A (en) * | 2021-01-28 | 2022-07-29 | 中国石油天然气股份有限公司 | Silicon-aluminum molecular sieve and preparation method thereof |
| CN113105356B (en) * | 2021-03-02 | 2023-10-03 | 浙江锦华新材料股份有限公司 | Preparation method of methoxyamine hydrochloride by coupling supergravity with ultrasound and microwaves |
| CN114870768B (en) * | 2022-04-01 | 2023-06-27 | 北京化工大学 | Molecular sieve synthesis system |
| CN114870663B (en) * | 2022-04-01 | 2023-08-08 | 北京化工大学 | Spiral-flow type hypergravity reactor |
| CN114733459B (en) * | 2022-04-01 | 2023-08-08 | 北京化工大学 | Heterogeneous nano dispersion strengthening reaction device and method |
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| CN101654257B (en) * | 2009-10-21 | 2011-10-26 | 中国铝业股份有限公司 | Method for preparing 4A zeolite by continuous crystallization |
| CN107224958B (en) * | 2016-03-23 | 2019-06-28 | 北京化工大学 | A kind of microwave coupling hypergravity swinging bed device and its application |
| CN205662326U (en) * | 2016-05-11 | 2016-10-26 | 中国石油大学(华东) | Overweight force method molecular sieve synthesizer |
| CN106564908B (en) * | 2016-11-14 | 2018-07-10 | 中北大学 | A kind of method that Impinging Stream-Rotating Packed Bed strengthens microwave synthesis ZSM-5 molecular sieve |
| CN108217674A (en) * | 2018-01-08 | 2018-06-29 | 北京化工大学 | A kind of hypergravity method for preparing Si-Al molecular sieve |
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| CN110078091B (en) * | 2019-04-26 | 2020-09-11 | 清华大学 | Complete method for continuously synthesizing titanium-silicon molecular sieve |
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