CN113083179A - Gas-liquid-solid three-phase supergravity reactor for coupling energy field and application - Google Patents
Gas-liquid-solid three-phase supergravity reactor for coupling energy field and application Download PDFInfo
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- CN113083179A CN113083179A CN202110229425.XA CN202110229425A CN113083179A CN 113083179 A CN113083179 A CN 113083179A CN 202110229425 A CN202110229425 A CN 202110229425A CN 113083179 A CN113083179 A CN 113083179A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
- B01F31/83—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations comprising a supplementary stirring element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C239/00—Compounds containing nitrogen-to-halogen bonds; Hydroxylamino compounds or ethers or esters thereof
- C07C239/08—Hydroxylamino compounds or their ethers or esters
- C07C239/20—Hydroxylamino compounds or their ethers or esters having oxygen atoms of hydroxylamino groups etherified
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00139—Controlling the temperature using electromagnetic heating
- B01J2219/00141—Microwaves
Abstract
The invention provides a hypergravity reactor applied to a coupling energy field of gas-liquid-solid three-phase reaction, which is provided with a first spiral unit, wherein the first spiral unit comprises a plurality of vertically arranged first columns, the gap and the width of each first column are in a micron level, and the spiral shape has the characteristics of high central density and low outer side density, so that the resistance at the tail end is smaller, and the gas-liquid-solid mass transfer/mixing effect is prevented from being poor due to liquid drop siltation and dropping. And the setting of stand can not hinder gaseous rising, and it is great that the spiral "blade" of dispersing simultaneously can make the liquid droplet resistance in center department, and outlying liquid droplet resistance is less, and then agrees with the speed of liquid injection in-process for the gas-liquid solid mass transfer of whole reactor/mix more evenly, gas-liquid solid reaction effect is more stable.
Description
Technical Field
The invention relates to the technical field of reactors. And more particularly, to a supergravity reactor for coupling energy fields for gas-liquid-solid three-phase reactions.
Background
At present, cutting components in the hypergravity reactor can be fillers or stators and rotors, and the like, and have a plurality of defects, and the preparation process of the methoxylamine hydrochloride has a plurality of problems, mainly has low etherification yield (less than or equal to 85 percent), has unknown side reaction, generates acetone by side reaction, and the like.
Content of application
In order to solve the defects, the invention provides a hypergravity reactor, which comprises:
the cutting device comprises a shell and a rotating cavity arranged in the shell, wherein a first cutting assembly and a liquid distributor positioned in the center of the cavity are arranged in the rotating cavity, and the first cutting assembly surrounds the outer side of the liquid distributor; the first cutting assembly comprises:
a plurality of first spiral units, each of which is arranged in a curved manner along a rotation direction of the rotary cavity, the first spiral units including a plurality of first cylinders arranged vertically along the spiral direction; wherein the content of the first and second substances,
the diameter of the first pillars and the width of the gap between any two adjacent first pillars in the plurality of first spiral units are both in the micrometer scale.
In a preferred embodiment, the diameter of the first pillars or the minimum gap width between any two adjacent first pillars in the plurality of spiral units is less than 2 microns.
In a preferred embodiment, a second cutting assembly is further disposed inside the rotary cavity, and the second cutting assembly includes:
the annular combination part can be sleeved on the first cutting assembly; and
a plurality of second spiral units, one end of each second spiral unit is fixed on the inner side wall of the annular combination part, and the other end of each second spiral unit is inserted into a gap between two adjacent first spiral units; the second spiral unit comprises a plurality of first columns which are vertically arranged along the spiral direction; wherein the content of the first and second substances,
the diameter of the second cylinder and the width of the gap between any two adjacent first cylinders in the spiral unit are both in the micrometer scale.
In a preferred embodiment, the diameter of the second cylinder or the minimum gap width between any two adjacent first cylinders in the plurality of spiral units is less than 2 microns.
In a preferred embodiment, the surfaces of the first cylinder and the second cylinder are oleophobic surfaces.
The invention further provides a system for preparing the methoxylamine hydrochloride by coupling the hypergravity with the ultrasound and the microwave, which comprises:
a first hypergravity circulation unit, a second hypergravity circulation unit, a heat exchange device and a refined ether unit, wherein,
the first hypergravity circulation unit is used for carrying out etherification reaction of acetone oxime in a hypergravity environment to generate acetone oxime methyl ether, the refined ether unit is used for carrying out refined ether process on the acetone oxime methyl ether, and the second hypergravity circulation unit is used for carrying out hydrolysis reaction on a refined ether product of the acetone oxime methyl ether and dilute hydrochloric acid in a hypergravity environment to generate methoxylamine hydrochloride;
the heat exchange device comprises a first heat exchanger and a second heat exchanger, the first heat exchanger is connected to the circulating pipeline of the first hypergravity circulating unit, and the second heat exchanger is connected to the circulating pipeline of the second hypergravity circulating unit;
the second hypergravity circulation unit comprises a hypergravity reactor as described above; and ultrasonic waves are fed into the first hypergravity circulation unit, and microwaves are fed into the second hypergravity circulation unit.
In a preferred embodiment, further comprising: an acetone condensation and collection unit;
the outlet of the fine ether unit is fine ether steam in a gas state, and the acetone condensation collection unit is communicated with the cavity for reaction in the second hypergravity circulation unit.
In a preferred embodiment, the first hypergravity circulation unit includes:
the system comprises a first hypergravity reactor and a first circulating tank which are communicated with each other, wherein an inlet of the first hypergravity reactor is connected with a reaction source pipeline, the first circulating tank is connected to the reaction source pipeline, and a first heat exchanger is connected to a pipeline between the first circulating tank and the reaction source pipeline.
In a preferred embodiment, the second hypergravity circulation unit further comprises:
and the second circulating tank is communicated with the second hypergravity reactor, a gas inlet of the second hypergravity reactor is connected with an outlet of the refined ether unit, an outlet of the second circulating tank is connected to the second hypergravity reactor and a pipeline connected with the refined ether unit, and the second heat exchanger is connected to an outlet pipeline of the second circulating tank.
In a preferred embodiment, further comprising:
the outlet of the first rectifying tower is communicated with the inlet of the refined ether unit; and the gas-liquid separation device is communicated with the outlet of the first rectifying tower.
The embodiment of the invention provides a supergravity reactor of a coupling energy field applied to gas-liquid-solid three-phase reaction, which comprises: a hypergravity reactor as described above, and an energy field feeder that can feed at least one energy field to the hypergravity reactor.
The invention has the following beneficial effects:
the invention provides a hypergravity reactor applied to a coupling energy field of gas-liquid-solid three-phase reaction, which is provided with a first spiral unit, wherein the first spiral unit comprises a plurality of vertically arranged first columns, the gap and the width of each first column are in a micron level, and the spiral shape has the characteristics of high central density and low outer side density, so that the resistance at the tail end is smaller, and the gas-liquid-solid mass transfer/mixing effect is prevented from being poor due to liquid drop siltation and dropping. And the setting of stand can not hinder gaseous rising, and it is great that the spiral "blade" of dispersing simultaneously can make the liquid droplet resistance in center department, and peripheral liquid droplet resistance is less, and then agrees with the speed in the liquid jet process for the gas-liquid solid mass transfer of whole reactor/mix more evenly, gas-liquid solid mass transfer/reaction effect is more stable.
Meanwhile, the key of the invention for finding the problems in the prior art is that heat is not removed in time, the invention combines the supergravity to carry out mass transfer and temperature control, and the heat exchanger continuously transfers heat in the reaction process, so that the heat in the production process of the product can be continuously removed, the generation of side reaction is avoided, the controllability and the enhancement of the multiphase reaction process are realized, in addition, the heat exchanger is innovatively coupled to the refined ether steam, and the acetone is stripped in the refined ether steam, so that the reaction separation coupling is realized.
Furthermore, according to the preparation system of methoxyamine hydrochloride by coupling the ultrasound with the microwaves, alkali liquor in the reaction can be uniformly distributed by dispersing alkali through ultrasound in the first supergravity circulation unit, so that the product is uniform, and the microwaves are coupled in the second supergravity circulation unit, so that the product can be uniformly heated through microwave enhanced heating.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows a schematic diagram of the preparation principle of methoxylamine hydrochloride in the prior art of the present invention.
Fig. 2 shows a schematic structural diagram of a methoxylamine hydrochloride preparation system in the prior art.
FIG. 3 shows a schematic structural diagram of a system for preparing methoxylamine hydrochloride by coupling supergravity with ultrasound and microwaves in the embodiment of the invention.
Fig. 4 shows a schematic structural diagram of a supergravity device in an embodiment of the present invention.
Fig. 5 shows a schematic structural diagram of the first spiral unit in the embodiment of the present invention.
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.
For a supergravity reactor, the filler needs to be wound layer by layer, liquid resistance is large for gas-liquid-solid mass transfer/mixing, so that liquid at the tail end cannot be cut due to small driving force, liquid drops cannot be sputtered due to excessively thick filler, and therefore the liquid drops are deposited and dropped at the tail end, so that the gas-liquid-solid mass transfer/mixing effect at the tail end is reduced, and similar problems also exist even if a stator and a rotor are used.
The present invention therefore provides a hypergravity reactor, as shown in fig. 4 and 5, comprising: the cutting device comprises a shell and a rotating cavity arranged in the shell, wherein a first cutting assembly and a liquid distributor positioned in the center of the cavity are arranged in the rotating cavity, and the first cutting assembly surrounds the outer side of the liquid distributor; the first cutting assembly comprises: a plurality of first spiral units, each of which is arranged in a curved manner along a rotation direction of the rotary cavity, the first spiral units including a plurality of first cylinders arranged vertically along the spiral direction; wherein the diameter of the first pillars and the width of the gap between any two adjacent first pillars in the plurality of first spiral units are both in the order of micrometers.
According to the supergravity reactor provided by the invention, the first spiral unit is arranged and comprises a plurality of vertically arranged first columns, the gaps and the widths of the first columns are in a micron level, and the spiral shape has the characteristics of high central density and low outer side density, so that the resistance at the tail end is smaller, and the gas-liquid-solid mass transfer/mixing effect is prevented from being poor due to liquid drops silting and dropping. And the setting of stand can not hinder gaseous rising, and it is great that the spiral "blade" of dispersing simultaneously can make the liquid droplet resistance in center department, and peripheral liquid droplet resistance is less, and then agrees with the speed in the liquid jet process for the gas-liquid solid mass transfer of whole reactor/mix more evenly, gas-liquid solid mass transfer/reaction effect is more stable.
In a preferred embodiment, the diameter of the first pillars or the minimum gap width between any two adjacent first pillars in the plurality of spiral units is less than 2 microns. In this embodiment, the 2 μm dimension can ensure that the resistance is within a reasonable range while the droplet is sufficiently sheared.
In a preferred embodiment, a second cutting assembly is further disposed inside the rotary cavity, and the second cutting assembly includes: the annular combination part can be sleeved on the first cutting assembly; and a plurality of second spiral units, one end of each second spiral unit is fixed on the inner side wall of the annular combination part, and the other end of each second spiral unit is inserted into a gap between two adjacent first spiral units; the second spiral unit comprises a plurality of first columns which are vertically arranged along the spiral direction; wherein the diameter of the second cylinder and the gap width between any two adjacent first cylinders in the spiral unit are both in the micrometer scale. The second spiral unit compensates for the problem of poor mixing effect caused by the excessively divergent ends.
In a preferred embodiment, the diameter of the second cylinder or the minimum gap width between any two adjacent first cylinders in the plurality of spiral units is less than 2 microns.
In a preferred embodiment, the surfaces of the first cylinder and the second cylinder are oleophobic surfaces.
The supergravity reactor provided by the invention can be applied to the following preparation process of methoxylamine hydrochloride.
The prior preparation process of methoxylamine hydrochloride has a plurality of problems, mainly has low etherification yield (less than or equal to 85%), has unknown side reaction, generates acetone and the like, as shown in figures 1 and 2, in the prior art process, a solvent, acetone oxime and alkali are added into a reaction kettle, methyl chloride is introduced, the temperature is controlled to be 20-60 ℃, the pressure is 0-0.1 MPa, the content of acetone oxime is detected to be less than or equal to 0.1% by center control analysis, and after the reaction is finished, the reaction liquid is subjected to reduced pressure rectification to obtain acetone oxime methyl ether. And hydrolyzing the acetone oxime methyl ether and dilute hydrochloric acid to obtain methoxylamine hydrochloride, and concentrating and crystallizing to obtain the final product.
The above process has the following problems:
(1) the etherification yield is low (less than or equal to 85 percent), unknown side reactions occur, and acetone is generated by the side reactions;
(2) sodium chloride and water are generated in the reaction, so that the whole reaction system is viscous, and the heat of etherification is difficult to remove (the reaction time of a 3m3 kettle is increased by 6 times compared with that of a 2L kettle);
(3) in the rectification period of the oxime methyl ether, if the content of ether in the kettle liquid is low, the temperature of the kettle liquid needs to be increased, the kettle liquid is easy to discolor at high temperature due to heat-sensitive impurities contained in the kettle liquid, and in addition, the process can also exist due to the fact that the solvent is recycled and water is removed;
(4) in the hydrolysis process of oxime methyl ether, the equilibrium of oxime ether-methoxy ammonium hydrochloride is established quickly, but the subsequent conversion rate is difficult to improve, and a large amount of oxime methyl ether is distilled out along with acetone (generally, the content of oxime methyl ether in a fraction exceeds 20%).
(5) The hydrolysis reaction liquid seriously corrodes the titanium material.
(6) The sodium chloride as a byproduct is difficult to be comprehensively utilized, and the product quality index of the sodium chloride is difficult to reach the sea salt standard except for incineration.
In view of the above, the first aspect of the present invention provides a system for preparing methoxylamine hydrochloride by coupling supergravity with ultrasound and microwave, comprising: the device comprises a first hypergravity circulation unit, a second hypergravity circulation unit, a heat exchange device and a refined ether unit, wherein the hypergravity circulation unit is used for carrying out an etherification reaction of acetone oxime in a hypergravity environment to generate acetone oxime methyl ether, the refined ether unit is used for carrying out a refined ether process on the acetone oxime methyl ether, and the second hypergravity circulation unit is used for carrying out a hydrolysis reaction on a refined ether product of the acetone oxime methyl ether and dilute hydrochloric acid in a hypergravity environment to generate methoxylamine hydrochloride; the heat exchange device comprises a first heat exchanger and a second heat exchanger, the first heat exchanger is connected to the circulating pipeline of the first hypergravity circulation unit, and the second heat exchanger is connected to the circulating pipeline of the second hypergravity circulation unit.
Wherein the second hypergravity circulation unit comprises a hypergravity reactor as described above.
And ultrasonic waves are fed into the first hypergravity circulation unit, and microwaves are fed into the second hypergravity circulation unit.
According to the system for preparing methoxyamine hydrochloride by coupling supergravity with ultrasound and microwaves, the key of the discovery of the invention is that heat is not removed in time, the invention combines supergravity to perform mass transfer and temperature control, and the heat exchanger continuously removes heat in the reaction process, so that the heat in the production process of products can be continuously removed, thereby avoiding side reaction generation, realizing the controllability and the enhancement of the multiphase reaction process, and innovatively coupling the heat exchanger to refined ether steam to perform acetone stripping by utilizing the refined ether steam in the refined ether steam, thereby realizing reaction separation coupling.
Furthermore, according to the preparation system of methoxyamine hydrochloride by coupling the ultrasound with the microwaves, alkali liquor in the reaction can be uniformly distributed by dispersing alkali through ultrasound in the first supergravity circulation unit, so that the product is uniform, and the microwaves are coupled in the second supergravity circulation unit, so that the product can be uniformly heated through microwave enhanced heating.
It is understood that the feeding of the microwave and the ultrasound according to the present invention may emit the microwave and the ultrasound toward the inside of the reactor through the microwave probe and the ultrasound probe, and adjust the output power through a power adjuster, that is, the intensity of the microwave and the ultrasound may be adjusted, and the microwave probe and the ultrasound probe are well known in the art and will not be described and illustrated herein.
It can be seen that in the system for preparing methoxyamine hydrochloride by coupling supergravity with ultrasound and microwave, due to the presence of the supergravity reactor, the stripping effect can be maximized, steam is more fully contacted with liquid drops during stripping, gas rising cannot be hindered by the arrangement of the upright columns, meanwhile, the divergent spiral blades can enable the liquid drop resistance at the center to be larger, the liquid drop resistance at the periphery to be smaller, and the speed in the liquid spraying process is matched, so that the gas-liquid-solid mass transfer/mixing of the whole reactor is more uniform, and the stripping effect is more stable.
The present invention will be described in detail with reference to the accompanying drawings.
Fig. 1 shows a schematic structural diagram of a system for preparing methoxyamine hydrochloride by coupling supergravity with ultrasound and microwaves in one embodiment of the present invention.
As shown in fig. 1, the embodiment shown in fig. 1 further includes: an acetone condensation and collection unit; the outlet of the fine ether unit is fine ether steam in a gas state, and the acetone condensation collection unit is communicated with the cavity for reaction in the second hypergravity circulation unit.
In the embodiment, the invention innovatively couples the heat exchanger to the refined ether steam, and the refined ether steam in the refined ether steam is utilized to strip acetone, so that the reaction separation coupling is realized.
Furthermore, the second supergravity reactor in the invention is the reactor with the spiral unit, due to the existence of the supergravity reactor, the stripping effect can be maximized, steam is more fully contacted with liquid drops during stripping, and the arrangement of the upright column can not obstruct gas rising, and the divergent spiral blade can ensure that the liquid drop resistance at the center is larger, the peripheral liquid drop resistance is smaller, and the speed in the liquid spraying process is matched, so that the gas-liquid-solid mass transfer/mixing of the whole reactor is more uniform, and the stripping effect is more stable.
In some embodiments, the first hypergravity cycle unit comprises: the system comprises a first hypergravity reactor and a first circulating tank which are communicated with each other, wherein an inlet of the first hypergravity reactor is connected with a reaction source pipeline, the first circulating tank is connected to the reaction source pipeline, and a first heat exchanger is connected to a pipeline between the first circulating tank and the reaction source pipeline.
The second hypergravity circulation unit includes: the second hypergravity reactor and the second circulation tank that communicate each other, the gas inlet of second hypergravity reactor and the exit linkage of smart ether unit, second circulation tank exit linkage to second hypergravity reactor with on the pipeline of smart ether unit connection, the second heat exchanger is connected on the outlet pipeline of second circulation tank.
It can be understood that the hypergravity reactor can shear liquid into liquid microelements with micro-nano scale, namely liquid films, liquid drops or liquid filaments with micro-nano scale.
In addition, the flow rate of the reaction gas source and the refined ether steam can be controlled by a pressure reducing valve and a flow dividing meter, and the invention is not described in detail.
In an embodiment of the present invention, the reaction gas comprises: methyl chloride, in an embodiment of the present invention, the reaction solution comprises: acetone oxime and alkali liquor enter the reaction system through a liquid inlet of the first hypergravity reactor.
Further, in practical use, a pressure gauge may be further provided, a pressure reducing valve may be provided on each pipe of the whole reaction system, and a flow meter and the like may be provided at a suitable position, which may be arbitrarily set according to specific requirements, which is not limited in the present invention.
The circulation of circulation tank and hypergravity reactor can provide power through the circulating pump, and the pump setting is between the pipeline of hypergravity reactor and circulation tank, with the liquid in the circulation tank and the solid catalyst pump of tiny particle go into hypergravity reactor, and the liquid in the hypergravity reactor flows to the circulation tank under the action of gravity, realizes the circulation.
It is understood that the high-gravity reactor can form a high-gravity field by means of high-speed centrifugation, namely, the centrifugal force is greater than 10g (earth gravity), and the gas, liquid and solid mass transfer/full shear dispersion can be realized by combining a cutting structure such as a filler, so that the mixing and mass transfer effects are greatly enhanced.
In order to adapt to preparation of methoxyamine hydrochloride, surfaces of the filler or the stator and the rotor can be subjected to oleophobic treatment to obtain oleophobic surfaces, so that influence of overhigh viscosity on the supergravity mixing effect is reduced.
In the preparation and use process of the methoxylamine hydrochloride provided by the invention, the detailed flow is as follows:
the flow is described as follows:
and (4) an etherification process. After the flake caustic soda is crushed and screened, the fine powder is taken to be fully mixed with the solvent and the acetone oxime in a circulating tank, and the mixture is pulped to be used as a reaction circulating material. The slurry is heated and recycled to preheat the reaction system. When the temperature rises to the specified temperature (60 ℃), methyl chloride is introduced for reaction. Because the reaction exotherm is large, heat needs to be continuously transferred through a heat exchanger in a circulating pipeline. After a certain period of reaction, the material was taken from the recycle tank for analysis.
② a hydrolysis process. Dilute hydrochloric acid is used as a bottom material, the temperature is raised, and the material is circularly heated in a reaction system. After the temperature rise value is set to a specified temperature, the refined ether and the dilute hydrochloric acid are mixed with the circulating material according to a certain proportion and then enter the super-gravity reactor for reaction. The acetone generated in the reaction process needs to be continuously removed to improve the conversion rate, and the test adopts the refined ether steam as the stripping gas to extract the generated acetone. Because the reaction process is a heat absorption process, heat is supplemented through a heat exchanger at the moment, and materials are taken out from the circulating tank for analysis after reaction for a period of time.
It will be appreciated that one of the core concepts of the present invention lies in the discovery of the cause of the occurrence of side reactions: the heat exchanger for heat transfer is coupled to a gas outlet of a circulating tank and a pipeline where the refined ether steam is located, and further the acetone is stripped by the refined ether steam, so that the reaction separation coupling is realized. It can be seen that the heat exchanger described above has a multiplexing effect.
Further, the method also comprises the following steps: the outlet of the first rectifying tower is communicated with the inlet of the refined ether unit; and the gas-liquid separation device is communicated with the outlet of the first rectifying tower.
Further, the first circulation tank and/or the inner wall of the first circulation tank is/are an oleophobic surface.
The key of the problem in the prior art is that heat is not removed in time, the mass transfer and temperature control are performed by combining the supergravity, and the heat is continuously removed by the heat exchanger in the reaction process, so that the heat can be continuously removed in the production process of the product, the generation of side reactions is avoided, the controllability and the enhancement of the multiphase reaction process are realized, and in addition, the heat exchanger is innovatively coupled to the refined ether steam, and the refined ether steam in the refined ether steam is utilized for stripping acetone, so that the reaction separation coupling is realized.
It can be understood that the supergravity reactor provided by the invention can be used for the above system, but is not limited to the above system, and those skilled in the art understand that the supergravity reactor provided by the invention can be used for most of gas-liquid, liquid-liquid, gas-liquid-solid, gas-solid and other reaction systems, and has certain universality. The core concept of the invention is that the structure of the filler is innovatively arranged, the first spiral unit is arranged and comprises a plurality of vertically arranged first columns, gaps and widths of the first columns are in a micron level, and the spiral shape has the characteristics of high central density and low outer side density, so that the resistance at the tail end is smaller, and the gas-liquid-solid mass transfer/mixing effect is prevented from being poor due to liquid drop silting and dropping. And the setting of stand can not hinder gaseous rising, and it is great that the spiral "blade" of dispersing simultaneously can make the liquid droplet resistance in center department, and peripheral liquid droplet resistance is less, and then agrees with the speed in the liquid jet process for the gas-liquid solid mass transfer of whole reactor/mix more evenly, gas-liquid solid mass transfer/reaction effect is more stable.
Based on this, another embodiment of the present invention provides a supergravity reactor for coupling energy fields applied to gas-liquid-solid three-phase reactions, including: a hypergravity reactor as described above, and an energy field feeder that can feed at least one energy field to the hypergravity reactor.
It can be understood that the supergravity reactor applied to the coupled energy field of the gas-liquid-solid three-phase reaction has the effects of the supergravity reactor and the coupled energy field, and the energy field may be an ultrasonic energy field, a microwave energy field, a magnetic field energy field, or the like, and the invention is not limited.
The terms "first," "second," and the like in the description and claims of the present invention and in the above-described drawings are used for distinguishing between different objects and not for describing a particular order. Furthermore, the terms "include" and "have," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, the inclusion of a list of elements, devices or systems is not limited to only those elements recited, but may alternatively include additional elements not listed, or may alternatively include additional elements, components, or the like inherent to such devices or systems.
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 (10)
1. A hypergravity reactor, comprising:
the cutting device comprises a shell and a rotating cavity arranged in the shell, wherein a first cutting assembly and a liquid distributor positioned in the center of the cavity are arranged in the rotating cavity, and the first cutting assembly surrounds the outer side of the liquid distributor; the first cutting assembly comprises:
a plurality of first spiral units, each of which is arranged in a curved manner along a rotation direction of the rotary cavity, the first spiral units including a plurality of first cylinders arranged vertically along the spiral direction; wherein the content of the first and second substances,
the diameter of the first pillars and the width of the gap between any two adjacent first pillars in the plurality of first spiral units are both in the micrometer scale.
2. The hypergravity reactor of claim 1, wherein,
the diameter of the first pillars or the minimum gap width between any two adjacent first pillars in the plurality of spiral units is less than 2 microns.
3. The hypergravity reactor of claim 1, wherein a second cutting assembly is further disposed inside the rotating chamber, the second cutting assembly comprising:
the annular combination part can be sleeved on the first cutting assembly; and
a plurality of second spiral units, one end of each second spiral unit is fixed on the inner side wall of the annular combination part, and the other end of each second spiral unit is inserted into a gap between two adjacent first spiral units; the second spiral unit comprises a plurality of first columns which are vertically arranged along the spiral direction; wherein the content of the first and second substances,
the diameter of the second cylinder and the width of the gap between any two adjacent first cylinders in the spiral unit are both in the micrometer scale.
4. The hypergravity reactor of claim 1, wherein,
the diameter of the second cylinder or the minimum gap width between any two adjacent first cylinders in the plurality of spiral units is less than 2 microns.
5. The hypergravity reactor of claim 3, wherein,
the surfaces of the first cylinder and the second cylinder are oleophobic surfaces.
6. A system for preparing methoxylamine hydrochloride by coupling supergravity with ultrasound and microwaves comprises:
a first hypergravity circulation unit, a second hypergravity circulation unit, a heat exchange device and a refined ether unit, wherein,
the first hypergravity circulation unit is used for carrying out etherification reaction of acetone oxime in a hypergravity environment to generate acetone oxime methyl ether, the refined ether unit is used for carrying out refined ether process on the acetone oxime methyl ether, and the second hypergravity circulation unit is used for carrying out hydrolysis reaction on a refined ether product of the acetone oxime methyl ether and dilute hydrochloric acid in a hypergravity environment to generate methoxylamine hydrochloride;
the heat exchange device comprises a first heat exchanger and a second heat exchanger, the first heat exchanger is connected to the circulating pipeline of the first hypergravity circulating unit, and the second heat exchanger is connected to the circulating pipeline of the second hypergravity circulating unit;
the second hypergravity circulation unit comprises the hypergravity reactor of any of claims 1 to 5; and ultrasonic waves are fed into the first hypergravity circulation unit, and microwaves are fed into the second hypergravity circulation unit.
7. The system for preparing the salt of hypergravity methoxyamine of claim 1, further comprising: an acetone condensation and collection unit;
the outlet of the fine ether unit is fine ether steam in a gas state, and the acetone condensation collection unit is communicated with the cavity for reaction in the second hypergravity circulation unit.
8. The system of claim 7, wherein the first hypergravity circulation unit comprises:
the system comprises a first hypergravity reactor and a first circulating tank which are communicated with each other, wherein an inlet of the first hypergravity reactor is connected with a reaction source pipeline, the first circulating tank is connected to the reaction source pipeline, and a first heat exchanger is connected to a pipeline between the first circulating tank and the reaction source pipeline.
9. The system of claim 7, wherein the second hypergravity circulation unit further comprises:
and the second circulating tank is communicated with the second hypergravity reactor, a gas inlet of the second hypergravity reactor is connected with an outlet of the refined ether unit, an outlet of the second circulating tank is connected to the second hypergravity reactor and a pipeline connected with the refined ether unit, and the second heat exchanger is connected to an outlet pipeline of the second circulating tank.
10. The utility model provides a solid three-phase hypergravity reactor of gas-liquid of coupling energy field and application which characterized in that includes: the hypergravity reactor of any of claims 1-5, and an energy field feeder that can feed at least one energy field to the hypergravity reactor.
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