CN218047836U - System for preparing epoxide by continuous flow micro-flux reactor - Google Patents

Abstract

The utility model relates to a chemical synthesis system field, concretely relates to system for preparation of epoxide by continuous flow micro-flux reactor. The system comprises a continuous flow micro-structure reactor, a liquid-liquid separator and an alkaline washing tower which are connected in sequence according to the material flow direction; wherein, one material inlet of the continuous flow microstructure reactor is connected with a solution A source which is used for providing a solution A containing a main catalyst, a peroxide stabilizer, hydrogen peroxide and water; the other material inlet is connected with a solution B source which is used for providing a solution B containing the substrate, the cocatalyst and the organic solvent; a material inlet of the liquid-liquid separator is connected with a material outlet of the continuous flow microstructure reactor; an organic phase outlet of the liquid-liquid separator is connected with a material inlet of the alkaline washing tower; the other material inlet of the alkaline tower is connected with an alkaline source which is used for providing alkaline aqueous solution. The system has high conversion rate, safety, high efficiency and environmental protection.

Description

System for preparing epoxide by continuous flow micro-flux reactor

Technical Field

The utility model relates to a chemical synthesis system field, concretely relates to system for little flux reactor preparation epoxide of continuous flow.

Background

The alicyclic epoxy resin and the condensate thereof have excellent comprehensive performances such as processability, thermal stability, electrical insulation, ultraviolet radiation resistance and the like because the alicyclic epoxy resin and the condensate thereof do not have residual chlorine and aromatic groups, and are widely applied to important industrial fields such as aerospace, microelectronic packaging, motor insulation and the like. In order to meet the increasing performance and functionalization requirements of modern industry on polymer materials, the synthesis and performance research of alicyclic epoxy resins has been actively carried out in recent years.

The alicyclic epoxy resin has determined molecular weight and molecular structure, various synthesis methods and strong structure designability, and the chemical structure of the alicyclic epoxy resin can be easily changed according to actual needs, so that the adjustment of the physical properties of the resin is realized. The physical property of the alicyclic epoxy resin is characterized in that the prior curing chamber is generally liquid and has lower viscosity, and the alicyclic epoxy resin can be directly used for construction operations such as coating, electronic packaging material and the like without being diluted by a solvent, and is convenient for technical operations such as encapsulation, pouring or vacuum injection and the like. The rigid structure of the alicyclic ring and the high crosslinking density of the cured product enable the alicyclic ring to have good bonding strength, high thermal deformation temperature, excellent chemical resistance and mechanical and electrical properties for different substrates. The alicyclic epoxy resin does not contain strong ultraviolet chromophoric groups such as aromatic rings and the like, and when the alicyclic epoxy resin is exposed to a high-voltage arc, micromolecular volatile matters such as carbon dioxide, carbon monoxide, water and the like are generated through decomposition, and a conductive path cannot be formed due to the generation of free carbon, so that the alicyclic epoxy resin has excellent high-voltage electricity leakage resistance. The excellent comprehensive performance enables the alicyclic epoxy resin to be applied in the fields of very large scale integrated circuit packaging, printed circuit board manufacturing, special light-cured coating, high-capacity and high-temperature resistant motor insulating materials for vacuum pressure impregnation technology and the like in recent years.

In the prior art, the method is that the alicyclic epoxy resin is prepared by adopting a traditional catalyst method, and the catalyst usually contains heavy metal ions (such as tungsten, molybdenum and the like), so that a reaction product also correspondingly contains a certain amount of heavy metal ion residues; because of the influence of the catalyst containing heavy metal ions, the final product also has heavy metal ion residues, and the trace amount of heavy metal ions also influence the curing speed (namely the gel time) of the product, so that the intramolecular cross-linking is influenced during curing, the gel time of the product is prolonged, and the production efficiency and the product quality are influenced; and the catalyst is usually high in price, cannot be recycled and is not beneficial to large-scale industrial production. The second method uses union carbide corporation peracid oxidation method, which adopts high-concentration peracid, the heat release is violent after the reaction is initiated, the residual peroxy groups are easy to gather, violent explosion can be caused after the reaction is triggered, and great potential safety hazard exists.

The prior art has the defects of incapability of continuously producing epoxy compounds, low conversion rate, poor safety, easiness in carrying heavy metal impurities, unsuitability for large-scale production and the like.

SUMMERY OF THE UTILITY MODEL

The present invention is directed to overcoming the above problems of the prior art and providing a system for continuous flow micro-flux production of epoxides. The utility model provides a system conversion rate is high, safety, high efficiency, environmental protection.

In order to achieve the above object, the present invention provides a system for preparing epoxide by using a continuous flow micro-flux reactor, which comprises a continuous flow micro-structure reactor, a liquid-liquid separator and an alkaline washing tower which are connected in sequence according to the material flow direction; wherein the content of the first and second substances,

one material inlet of the continuous flow microstructure reactor is connected with a solution A source, and the solution A source is used for providing a solution A containing a main catalyst, a peroxide stabilizer, hydrogen peroxide and water; the other material inlet is connected with a solution B source which is used for providing a solution B containing the substrate, the cocatalyst and the organic solvent;

a material inlet of the liquid-liquid separator is connected with a material outlet of the continuous flow microstructure reactor;

an organic phase outlet of the liquid-liquid separator is connected with a material inlet of the alkaline washing tower; the other material inlet of the alkaline tower is connected with an alkaline source, and the alkaline source is used for providing alkaline aqueous solution; so that the material from the liquid-liquid separator is quenched by the action of alkali in the caustic tower.

In one example, the system further comprises a concentration and crystallization unit, wherein a material inlet of the concentration and crystallization unit is connected with the alkaline aqueous solution separated from the alkaline tower and the acidic aqueous solution led out from the liquid-liquid separator, so that the alkaline aqueous solution and the acidic aqueous solution react in the concentration and crystallization unit and are concentrated and crystallized to obtain the byproduct containing the main catalyst.

In one example, the system further comprises a cleaning unit connected to the organic material outlet of the caustic tower for washing reaction products in the material of the organic material outlet of the caustic tower.

In one example, the wash unit is a water wash column.

In one example, the inlet of the water wash tower is connected to the organic phase outlet of the caustic wash tower; the other inlet of the water washing tower is connected with a water source; the water phase outlet of the water washing tower is connected with the water phase inlet of other equipment needing water.

In one example, the system further comprises a purification unit connected to the organic material outlet of the washing unit, the purification unit for purifying the reaction product.

In one example, the purification unit comprises a primary thin film evaporator and a secondary thin film evaporator connected in series for purifying the material from the water wash column.

In one example, the purification unit further comprises a condenser connected to the gas phase outlet of the primary thin film evaporator and the gas phase outlet of the secondary thin film evaporator, respectively, for condensing the solvent and collecting the condensed solvent into a solvent tank.

In one example, the system further comprises connecting the solvent collected in the solvent tank to other equipment requiring the use of an organic solvent.

In one example, the system further comprises a control module for controlling operation of the system.

Compared with the prior art, the beneficial effects of the utility model are that:

(1) The utility model adopts the characteristics of the continuous flow micro-flux reactor, has small effective liquid holdup and serialization, can realize sufficient mixing and high-efficiency heat transfer in a short time, greatly shortens the reaction time, and simultaneously effectively improves the product conversion rate and selectivity, therefore, the utility model is a safe, high-efficiency and environment-friendly continuous flow production process;

(2) The utility model adopts the clear reaction liquid obtained by the working procedures of liquid separation, quenching and cleaning of the reaction liquid flowing out from the continuous flow micro-flux reactor through a liquid-liquid separator, a continuous alkaline washing tower and a continuous water washing tower, and enters a first-stage film evaporator and a second-stage film evaporator to obtain finished products;

(3) The utility model can realize full-automatic or semi-automatic continuous operation by the series connection of the processes of reaction, phase splitting, quenching, cleaning, purification and the like and the reasonable distribution of flow, thereby greatly improving the production efficiency; then, a combined control system and a continuous flow process are adopted, so that the temperature runaway phenomenon in the reaction process is avoided, and the safety and the stability of the whole process can be realized;

(4) The utility model discloses the buck that produces at the quenching in-process can with the concentrated sour aquatic in the liquid-liquid separation step with, catalyst solution repeatedly usable who obtains after concentrating washs water also circulated use in the quenching process, and the solvent of purification process can be applied mechanically, has realized the cyclic utilization of resource, green.

The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.

Drawings

FIG. 1 is a schematic diagram of an exemplary epoxidation reaction system.

Description of the reference numerals

P-1, a first delivery pump; p-2, a second delivery pump; r-1, a continuous flow microstructure reactor; s-1, a liquid-liquid separator; t-1, an alkaline washing tower; t-2, washing a tower with water; e-1, a first condenser; e-2, a second condenser; e-3, a third condenser; d-1, a first-stage thin film evaporator; d-2, a secondary film evaporator; c-1, a finished product tank; c-2, a solvent tank.

Detailed Description

The present invention will be described in detail below by way of examples. The embodiments described herein are only some embodiments, not all embodiments, of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

The system according to one embodiment is shown in fig. 1, and the system shown in fig. 1 can be divided into the operation steps of continuous reaction, liquid separation, quenching, washing, purification and the like. The system is described below in an exemplary manner in conjunction with the figures.

In one example, the system comprises a continuous flow micro-structure reactor R-1, a liquid-liquid separator S-1 and an alkaline tower T-1 which are connected in sequence according to the material flow direction; wherein, the first and the second end of the pipe are connected with each other,

one material inlet of the continuous flow microstructure reactor R-1 is connected with a solution A source, and the solution A source is used for providing a solution A containing a main catalyst, a peroxide stabilizer, hydrogen peroxide and water; the other material inlet is connected with a solution B source which is used for providing a solution B containing the substrate, the cocatalyst and the organic solvent;

a material inlet of the liquid-liquid separator S-1 is connected with a material outlet of the continuous flow micro-structure reactor R-1;

an organic phase outlet of the liquid-liquid separator S-1 is connected with a material inlet of the alkaline washing tower T-1; the other material inlet of the alkaline washing tower T-1 is connected with an alkali source, and the alkali source is used for providing an alkaline aqueous solution; so that the material from the liquid-liquid separator S-1 is quenched by the action of alkali in the alkaline tower T-1.

The continuous flow microstructure reactor R-1 can be selected from the types of microchannel reactors, micro-tube reactors, tubular reactors and the like independently, and the microstructure reactor can be selected from the commercial brands and can also be selected to be customized. The material of the reactor is not limited to non-metallic materials such as quartz, glass, and silicon carbide, and is not limited to metallic materials such as stainless steel.

The continuous flow microstructured reactor R-1 is particularly suitable for use in the production of epoxides where heterogeneous reactions are present, compared to reactors conventionally used in the prior art. And the inventor of the utility model further rearranges the reaction method and system, effectively improving the conversion rate, selectivity, product quality and yield of the reaction.

And in the continuous flow microstructure reactor R-1, the solution A and the solution B enter in parallel and perform continuous reaction, and the obtained material is the material containing the final target product.

The reactions and reaction feeds used in the continuous flow microstructure reactor R-1 can be the same as is conventional in the art for the preparation of epoxides. The following is an exemplary illustration of reaction materials more suitable for use in the systems and methods of the present invention.

In one example, the solution a is obtained by dissolving a peroxide stabilizer and a procatalyst in an aqueous hydrogen peroxide solution.

In one example, the solution B is obtained by dissolving the substrate and the cocatalyst in an organic solvent.

In one example, the peroxide stabilizer is one or more of sodium phosphate, sodium dipolyphosphate, sodium tripolyphosphate, and sodium polyphosphate.

In one example, the peroxide stabilizer concentration in solution a is 0.1-1%.

In one example, the procatalyst is an organic base, an inorganic base or a basic salt, and the organic base or strong base weak acid salt includes one or more of dimethylamine, triethylamine, ammonia, sodium hydroxide, potassium hydroxide, sodium acetate, potassium acetate, ammonium acetate, sodium bicarbonate, sodium carbonate, potassium bicarbonate, sodium dihydrogen phosphate, sodium monohydrogen phosphate, potassium dihydrogen phosphate, and potassium monohydrogen phosphate.

In one example, the substrate is a cyclohexene-based organic.

In one example, the organic solvent is one or more of an aromatic hydrocarbon solvent, a halogenated hydrocarbon solvent, or an ester solvent.

In one example, the helper catalyst comprises an organic acid or anhydride.

In one example, the aqueous hydrogen peroxide solution has a concentration of 30-70%.

The amount of each material in the solution A and the solution B is related to the amount of the substrate added.

In one example, the mass ratio of substrate to organic solvent is 1 (1-4).

In one example, the equivalent ratio of the substrate to the co-catalyst (the term "equivalent ratio" means the molar ratio of the respective species) is 1 (1-5).

In one example, the equivalent ratio of the substrate to the hydrogen peroxide is 1 (1.5-4).

In one example, the reaction conditions in the continuous flow microstructure reactor may be set according to the needs of the reaction, for example, the conditions of the continuous flow microstructure reactor may include: the temperature is 40-90 deg.C, and the time is 30-600s.

The system can also be provided with a plurality of delivery pumps according to the requirement. For example, a first delivery pump P-1 for delivering the solution A, and a second delivery pump P-2 for delivering the solution B may be included.

The liquid-liquid separator S-1 further comprises a water phase outlet, and the water phase outlet outputs an acidic aqueous solution.

The quenching unit is used for quenching the reaction of the materials from the liquid-liquid separator S-1. The quenching unit mainly comprises a caustic washing tower T-1. The caustic washing tower T-1 may use a commercially available caustic washing tower which is conventional in the art.

The material in the caustic tower T-1 is separated into an organic phase and an aqueous phase, wherein the organic phase enters the cleaning unit.

In an example, the system further comprises a concentration and crystallization unit, a material inlet of the concentration and crystallization unit is connected with the alkaline aqueous solution separated from the alkaline tower T-1 and the acidic aqueous solution led out from the liquid-liquid separator S-1, the concentration and crystallization unit comprises a neutralization device, a concentration device, a crystallization device and a filtration device which are connected in sequence, wherein the material inlet of the neutralization device is connected with the aqueous phase outlet of the liquid-liquid separator S-1 to input the acidic aqueous solution, and the material inlet of the neutralization device is also connected with the aqueous phase outlet of the alkaline tower T-1 to input the alkaline aqueous solution, so that the acidic aqueous solution and the alkaline aqueous solution react in the neutralization device, and the obtained product is sequentially concentrated in the concentration device, crystallized in the crystallization device, filtered in the filtration device, and dried in a drying device to finally obtain the byproduct containing the main catalyst. The liquid-liquid separator S-1 can also comprise a gas phase outlet which is connected with the outside or a subsequent treatment process.

The continuous flow microstructure reactor R-1 is the main generation place of epoxidation reaction; the liquid-liquid separator S-1 is a main place for liquid separation; the concentration and crystallization unit is a main generation place for recovering the by-product containing the main catalyst.

And the solution A source and the solution B source respectively enter the continuous flow micro-structure reactor R-1 through the first conveying pump P-1 and the second conveying pump P-2 to react, materials flowing out of the continuous flow micro-structure reactor R-1 are conveyed to the liquid-liquid separator S-1 to carry out liquid-liquid phase separation, and the acidic aqueous solution after phase separation is contacted with the alkaline aqueous solution in the subsequent alkali washing step and then sequentially passes through a neutralization device, a concentration device, a crystallization device and a filtering device to be neutralized, concentrated, crystallized and filtered to obtain a byproduct containing the main catalyst. And after the acidic organic phase is conveyed to the alkaline tower T-1, carrying out quenching reaction with an alkaline aqueous solution in the alkaline tower T-1, feeding the alkaline water separated after quenching into the neutralization step, and feeding the organic phase separated after quenching into a subsequent cleaning step.

In one embodiment, the system further comprises a cleaning unit connected to the organic material outlet of the caustic tower T-1 for washing reaction products in the material of the organic material outlet of the caustic tower T-1.

In one embodiment, the washing unit is a water wash column T-2. The water washing column T-2 may use a commercially available water washing column conventional in the art.

The material of the water wash column T-2 is separated into an organic phase and an aqueous phase, wherein the organic phase enters the purification unit.

In one embodiment, the inlet of the water scrubber T-2 is connected to the organic phase outlet of the caustic scrubber T-1; the other inlet of the water washing tower T-2 is connected with a water source; and the water phase outlet of the water washing tower T-2 is connected with the water phase inlet of other equipment needing water.

And (3) continuously feeding the alkaline aqueous solution separated from the alkaline tower T-1 into the water scrubber T-2, and cleaning in the water scrubber T-2 to remove water-soluble impurities in an organic phase.

In one embodiment, the system further comprises a purification unit coupled to the organic material outlet of the washing unit for purifying the reaction product to obtain a final epoxide product.

In one embodiment, the purification unit comprises a primary thin film evaporator D-1 and a secondary thin film evaporator D-2 connected in series for purifying the feed from the water wash column T-2. The purified material enters a finished product tank C-1 for collection; the purification unit further comprises condensers (such as a first condenser E-1 and a second condenser E-2 connected to the primary thin film evaporator D-1 and a third condenser E-3 connected to the secondary thin film evaporator D-2) respectively connected to the gas phase outlets of the primary thin film evaporator D-1 and the secondary thin film evaporator D-2 for condensing and collecting the solvent, and the collected solvent is stored in a solvent tank C-2.

In one embodiment, the system further comprises connecting the solvent collected in the solvent tank C-2 with other equipment requiring the use of organic solvent to recycle the organic solvent.

The organic phase flowing out in the cleaning step sequentially enters the primary film evaporator D-1 and the secondary film evaporator D-2 to remove impurities such as residual organic solvent and the like, the organic gas generated by the primary film evaporator D-1 sequentially passes through a first condenser E-1 and a second condenser E-2, the organic gas generated by the secondary film evaporator D-2 passes through a third condenser E-3, the organic gas is condensed by the condensers and then enters a solvent receiving tank, and the heavy component flowing out of the secondary film evaporator D-2 is separated into a finished product tank C-1.

The purification unit may also include other equipment conventional in the art, such as a crude receiver tank, a transfer pump, and a heavies receiver tank, such that: pumping the continuously separated clarified reaction liquid into a first-stage film evaporation device area, pumping the solvent into a solvent receiving tank through a first condenser and a second condenser, pumping the crude product into a second-stage film evaporation device area through a first material transferring pump, pumping the light component into the solvent receiving tank through a third condenser, and separating the heavy component into a finished product tank.

In the primary thin film evaporator D-1, the conditions for thin film evaporation thereof include: the temperature is 60-100 ℃; the vacuum degree is 50-1000Pa.

In the secondary thin film evaporator D-2, conditions for the secondary thin film evaporation thereof include: the temperature is 100-130 ℃; the vacuum degree is 5-100Pa.

Through twice distillation, the solvent can be completely removed, and the impurity residues are also effectively removed after the product is distilled, so that the product quality is greatly improved, and the stability of the product is improved.

In order to achieve maximum resource utilization and green production, the system preferably further comprises a recycling or recycling process.

The recovery or recycle treatment may comprise at least one of the following operations:

the first operation: reacting the alkaline aqueous solution separated after quenching with the acidic aqueous solution separated after extraction to obtain a byproduct containing the main catalyst;

and operation II: the alkaline aqueous solution separated after washing is used for quenching;

operation three: using the separated organic solvent after purification in the operation needing to use the organic solvent in the system;

and operation four: the aqueous solution separated after concentration, quenching or washing in the system is used in operations requiring the use of water in the system.

The first operation is a recovery operation, and byproducts can be obtained to realize additional economic value. The specific mode comprises the following steps: at least part of the alkaline aqueous solution separated after quenching reacts with the acidic aqueous solution separated after extraction, so as to generate a pre-recovered by-product of the target main catalyst, and the by-product of the main catalyst can be finally obtained through further treatment (such as concentration, crystallization, filtration and the like).

The second operation is a circulating operation, so that the alkaline aqueous solution can be recycled in the system. The specific mode comprises the following steps: at least part of the alkaline aqueous solution separated after washing is used for reaction quenching; and/or as a water source in other steps.

The third operation is a circulating operation, so that the organic solvent can be recycled in the system. The concrete method comprises the following steps: the organic solvent separated after purification is used in operations in the system that require the use of an organic solvent, for example for extraction and/or for the preparation of solution B.

And the fourth operation is a circulating operation, so that water can be recycled in the system. The specific mode comprises the following steps: the aqueous solution separated after concentration, quenching or washing in the system is used in operations requiring the use of water in the system.

Thereby the utility model discloses can realize the maximize of resource, quench the alkaline water of separation and extract the acidic water neutralization of separation, through concentration, crystallization, filtration, can obtain the main catalyst that contains crystal water, through the packing back, sell as the byproduct. The water separated by washing can be used as a water source for a quenching process, and the water concentrated by neutralization can be used as a water source for a washing process; the solvent recovered in the purification process can be recycled.

Each step and operation of the system can be continuously carried out or semi-continuously carried out.

In one embodiment, the system further comprises a control module for controlling the operation of the system. Therefore, through the series connection of the processes of continuous reaction, liquid separation, quenching, cleaning, purification and the like, and through the reasonable distribution of flow, the full-automatic or semi-automatic continuous operation can be realized, and the production efficiency is greatly improved; and then, a joint control system and a continuous flow process are adopted, so that the temperature runaway phenomenon in the reaction process is avoided, and the safety and the stability of the whole process can be realized. The intelligent control system can realize serialization, miniaturization, sealing, automation and modularization, and finally can realize the intelligence of autonomous learning and control through modeling and algorithm if modules such as online detection and data monitoring are added.

The system can be carried out through the control module, can detect and regulate and control each link of each device, and can obtain reasonable flow in each part through calculation so as to continuously and smoothly carry out the reaction.

Compared with the prior art, the system of the utility model has the following advantages at least:

1) The utility model discloses a characteristics of continuous flow micro flux reactor, effective liquid holdup is little, and the serialization can realize fully mixing in the short time and high-efficient heat transfer, and very big when having shortened the reaction is long, effectively improves product conversion rate and selectivity simultaneously, consequently the utility model discloses a continuous flow production technology of safety, high efficiency, environmental protection.

(2) The utility model discloses a reaction liquid that continuous flow micro flux reactor flows realizes separating liquid, quenching, the clarification reaction liquid that the cleaning process obtained through liquid-liquid separator, continuous alkaline wash tower, continuous washing tower, gets into one-level film evaporator, second grade film evaporator and obtains the finished product.

(3) The utility model can realize full-automatic or semi-automatic continuous operation by the series connection of the processes of reaction, phase splitting, quenching, cleaning, purification and the like and the reasonable distribution of flow, thereby greatly improving the production efficiency; and then, a joint control system and a continuous flow process are adopted, so that the temperature runaway phenomenon in the reaction process is avoided, and the safety and the stability of the whole process can be realized.

(4) The utility model discloses the buck that produces at the quenching in-process can with the concentrated sour aquatic in the liquid-liquid separation step with, catalyst solution repeatedly usable who obtains after concentrating washs water also circulated use in the quenching process, and the solvent of purification process can be applied mechanically, has realized the cyclic utilization of resource, green.

Examples

The system for preparing epoxide as shown in figure 1 comprises at least the following steps:

(1) Reaction: the prepared solution A and solution B are respectively and accurately pumped into a continuous flow micro-flux structure reactor R-1 through a first delivery pump P-1 and a first delivery pump P-2 to carry out continuous epoxidation reaction.

(2) Separation: reaction liquid flowing out of the continuous flow micro-flux structure reactor R-1 enters the liquid-liquid separator S-1 through reasonable flow control, separation of a water phase and an organic phase is achieved in the liquid-liquid separator S-1, the separated acidic organic phase enters the alkaline tower T-1 and reacts with alkaline water to achieve quenching, the separated acidic aqueous solution contacts with the separated alkaline aqueous solution after quenching of the alkaline tower T-1 and then is subjected to subsequent neutralization, concentration, crystallization and filtration operation steps, so that a main catalyst in the reaction is recovered, and recycling of the catalyst is achieved. The organic phase separated from the alkaline tower T-1 enters a water scrubber T-2 for cleaning, the water phase separated from the water scrubber T-2 can be used in other steps needing water in the system, and the three steps of phase separation, quenching and cleaning are realized through the steps by the reaction liquid continuously (semi-continuously) passing through a liquid-liquid separator, a continuous alkaline tower and a continuous water scrubber, so that the clear reaction liquid is obtained.

(3) And (3) purification: clear reaction liquid flowing out of the water washing tower T-2 sequentially enters a primary thin film evaporator D-1 and a secondary thin film evaporator D-2 through reasonable flow control, gas phase coming out of the primary thin film evaporator D-1 enters a first condenser E-1 and a second condenser E-2 to be condensed and then enters a solvent receiving tank C-1, gas phase coming out of the secondary thin film evaporator D-2 enters a third condenser E-1 to be condensed and then enters the solvent receiving tank C-1, heavy components flowing out of the secondary thin film evaporator D-2 are separated into a finished product tank C-1, and purification process operation is achieved through the steps, and finished products are obtained.

(4) Resource maximization: the embodiment also embodies the cyclic utilization of resources, and specifically embodies the following aspects: and (3) neutralizing and concentrating the alkaline water obtained by quenching separation and the acidic water obtained by liquid-liquid separation to obtain a saturated solution of the catalyst, and filtering the crystallized water-containing catalyst after crystallization to obtain the crystal water-containing catalyst which can be used for preparing the solution A, wherein the surplus crystal water can also be sold as a byproduct. The water separated in the concentration, quenching and washing processes can be reused, wherein the water separated in the concentration process can be used in the washing process, and the water separated in the washing process can be used in the quenching process. The solvent recovered in the purification step can be continuously recycled.

The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. In the technical concept scope of the present invention, it can be right to perform multiple simple modifications to the technical solution of the present invention, including each technical feature combined in any other suitable manner, these simple modifications and combinations should be considered as the disclosed content of the present invention, all belonging to the protection scope of the present invention.

Claims (9)

1. The system for preparing the epoxide by the continuous flow micro-flux reactor is characterized by comprising a continuous flow micro-structure reactor, a liquid-liquid separator and an alkaline tower which are connected in sequence according to the material flow direction; wherein, the first and the second end of the pipe are connected with each other,

one material inlet of the continuous flow microstructure reactor is connected with a solution A source, and the solution A source is used for providing a solution A containing a main catalyst, a peroxide stabilizer, hydrogen peroxide and water; the other material inlet is connected with a solution B source which is used for providing a solution B containing the substrate, the cocatalyst and the organic solvent;

a material inlet of the liquid-liquid separator is connected with a material outlet of the continuous flow micro-structure reactor;

an organic phase outlet of the liquid-liquid separator is connected with a material inlet of the alkaline washing tower; the other material inlet of the alkaline tower is connected with an alkaline source, and the alkaline source is used for providing alkaline aqueous solution; so that the material from the liquid-liquid separator is quenched by the action of alkali in the caustic tower.

2. The system as claimed in claim 1, further comprising a concentration crystallization unit, wherein the material inlet of the concentration crystallization unit is connected with the alkaline aqueous solution separated from the alkaline tower and the acidic aqueous solution led out from the liquid-liquid separator, so that the alkaline aqueous solution and the acidic aqueous solution react in the concentration crystallization unit and are concentrated and crystallized to obtain the byproduct containing the main catalyst.

3. The system of claim 1, further comprising a cleaning unit connected to the organic material outlet of the caustic tower, the cleaning unit configured to wash reaction products in the material of the organic material outlet of the caustic tower.

4. The system of claim 3, wherein the washing unit is a water wash tower.

5. The system according to claim 4, wherein an inlet of the water wash tower is connected to an organic phase outlet of the caustic wash tower; the other inlet of the water washing tower is connected with a water source; the water phase outlet of the water washing tower is connected with the water phase inlet of other equipment needing water.

6. The system of claim 4, further comprising a purification unit connected to the organic material outlet of the washing unit, the purification unit configured to purify the reaction product.

7. The system of claim 6, wherein the purification unit comprises a primary thin film evaporator and a secondary thin film evaporator connected in series for purifying the material from the water wash column.

8. The system of claim 7, wherein the purification unit further comprises a condenser connected to the gas phase outlets of the primary and secondary thin film evaporators, respectively, for condensing the solvent and collecting it into a solvent tank.

9. The system of claim 8, further comprising connecting the solvent collected in the solvent tank to other equipment requiring the use of organic solvents.

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