CN110156724B - Device and method for preparing epoxy compound by batch reaction - Google Patents
Device and method for preparing epoxy compound by batch reaction Download PDFInfo
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- CN110156724B CN110156724B CN201910549058.4A CN201910549058A CN110156724B CN 110156724 B CN110156724 B CN 110156724B CN 201910549058 A CN201910549058 A CN 201910549058A CN 110156724 B CN110156724 B CN 110156724B
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- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
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Abstract
The invention provides a device and a method for preparing an epoxy compound by batch reaction. The device integrates the reaction and separation processes into the same unit, the combination of the reactor and the separator plays an important role in the reaction efficiency, and the device is suitable for the synthesis of various epoxy compounds, the conditions are mild, and the risk coefficient is small; the method has high efficiency and high yield and selectivity of the epoxy compound.
Description
Technical Field
The invention belongs to the technical field of organic synthesis, and relates to a device and a method for preparing an epoxy compound by an intermittent reaction.
Background
Epoxy compounds are a class of compounds having a ternary cyclic ether structure, the simplest of which is ethylene oxide. Like cyclopropane, epoxy compounds have a high ring tension of 114.1kJ/mol, are chemically very reactive and can react with a wide variety of compounds. Representative examples of the epoxy compound include ethylene oxide, propylene oxide, 1, 2-epoxybutane, 2, 3-epoxybutane, 1, 2-epoxypentane, 2, 3-epoxypentane and the like. The epoxy compounds have large market demand and are important organic chemical products, however, the preparation technology of only simple epoxy compounds such as ethylene oxide, propylene oxide and the like is mature at present, and other epoxy compounds with large molecular weight still have a plurality of difficulties.
At present, the production routes of epoxy compounds mainly include direct oxidation and indirect oxidation. CN 104650008A discloses a process and a system for preparing propylene oxide by directly oxidizing propylene with oxygen and hydrogen, wherein propylene, circulating propylene and high boiling point organic sulfide are added into a mixed solvent of methanol and hydrazine hydrate, hydrogen and oxygen are introduced to generate a crude product of propylene oxide, the crude product sequentially passes through a crude separation tower and a propylene stripping tower, and the residual mixed solution of propylene oxide enters an extraction and purification tower containing cumene and alkaline solution for further extraction and rectification to obtain a high-purity propylene oxide product. CN 108947938A discloses a process for the production of propylene oxide by subjecting a stream comprising ethane to oxidative dehydrogenation conditions to produce ethylene, subjecting said stream comprising ethylene and unconverted ethane to oxidative conditions to produce ethylene oxide, producing a stream comprising ethylene oxide, unconverted ethylene and ethane, and recovering and separating ethylene oxide from this stream. However, the oxidation method for preparing epoxy compounds at present requires harsh conditions, is easy to explode, and does not meet the requirements of safe production, so researchers also continuously develop new methods for preparing epoxy compounds.
The thermal decomposition method is a common method for preparing inorganic materials, is less applied to organic matters, and is a new method which is worth researching by reversely preparing epoxy compounds from products thereof according to reactions which can occur to the epoxy compounds so as to solve the problems of complicated steps, difficult separation and low safety in the existing method.
Disclosure of Invention
The invention aims to provide a device and a method for preparing epoxy compounds by batch reaction, which take epoxy carbonate as a raw material, prepare the epoxy compounds by a decomposition method, and integrate the reaction and separation processes into a reaction separation unit for carrying out, thereby not only improving the yield of products, but also simplifying the process flow; the method is suitable for various epoxy compounds, and the reaction conditions are mild.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides an apparatus for preparing an epoxy compound by a batch reaction, the apparatus comprising a reaction separation unit, a product collection unit, a vacuum control unit and a recovery unit, wherein an upper outlet of the reaction separation unit is connected with the product collection unit, the product collection unit is connected with the vacuum control unit, and a lower outlet of the reaction separation unit is connected with the recovery unit.
According to the invention, the device is used for preparing the epoxy compound, each unit and the connection relation thereof in the device are selected according to the reactant and the reaction type, the reaction and the separation are integrated into one unit, the reaction product is separated from the reactant in time, the forward proceeding of the reaction is facilitated, the conversion rate of the reactant is improved, the number of the devices can be reduced, and the cost is reduced.
The following technical solutions are preferred but not limited to the technical solutions provided by the present invention, and the technical objects and advantages of the present invention can be better achieved and realized by the following technical solutions.
As a preferred technical scheme of the invention, the reaction separation unit comprises a reactor and a separator, and the reactor and the separator are in the same equipment or belong to different equipment.
Preferably, the reactive separation unit comprises any one of a tank reactor, a membrane reactor, a column reactor or a tubular reactor, or a combination of at least two of these, typical but non-limiting examples being: the combination of a kettle reactor and a membrane reactor, the combination of a membrane reactor and a tower reactor, the combination of a kettle reactor, a tower reactor and a tubular reactor, and the like.
In the invention, the reaction separation unit is formed by integrating the reactor and the separator, the reactor and the separator can be in the same equipment, and the reaction and separation operations are only distinguished at the moment, for example, in a kettle type reactor, a reboiler, a tower kettle or a certain tower plate, rising steam is a reaction product; it is also possible that the two are not in the same apparatus, such as a combination of a tubular reactor and a thin film evaporator which is capable of separating the reaction product from the reactants. The combination of the reactor and the separator, depending on the type of reactor chosen, has a significant influence on the efficiency of the reaction.
As a preferred technical solution of the present invention, the tank reactor comprises any one or a combination of at least two of an internal loop reaction kettle, an internal gas circulation reaction kettle, an internal catalyst holder reaction kettle, an internal baffle reaction kettle and an external forced circulation system reaction kettle, and the combination is typically but not limited to: the reactor comprises a combination of an internal circulation reaction kettle and an internal gas circulation reaction kettle, a combination of an internal catalyst fixer reaction kettle and an internal baffle reaction kettle, a combination of an internal circulation reaction kettle, an internal catalyst fixer reaction kettle and a reaction kettle of an external forced circulation system, and the like.
Wherein, the forced circulation system arranged outside the reaction kettle comprises functional components such as an external heat exchanger, an external tubular reactor, a rectifying column and the like.
Preferably, the membrane reactor comprises any one of or a combination of at least two of a falling film reactor, a rising film reactor or a wiped film reactor, typical but non-limiting examples of which are: the combination of a falling film reactor and a rising film reactor, the combination of a rising film reactor and a wiped film reactor, the combination of a falling film reactor, a rising film reactor and a wiped film reactor and the like.
Preferably, the column reactor comprises any one of a packed column, a float valve column or a sieve plate column, or a combination of at least two of these, typical but non-limiting examples being: the combination of a packed tower and a float valve tower, the combination of a float valve tower and a sieve plate tower, the combination of a packed tower, a float valve tower and a sieve plate tower and the like.
Preferably, the tubular reactor comprises any one of a single tubular reactor, a multi-tubular reactor, a forced plug flow tubular reactor or a forced back-mixed tubular reactor or a combination of at least two of these, typical but non-limiting examples being: the combination of a single-tube reactor and a multi-tube reactor, the combination of a forced plug flow tube reactor and a forced back-mixed tube reactor, the combination of a single-tube reactor, a multi-tube reactor and a forced plug flow tube reactor, and the like.
In the invention, the device also comprises a premixing unit, and the premixing unit is connected with the reaction separation unit.
In another aspect, the present invention provides a method for preparing an epoxy compound using the above apparatus, the method comprising: heating raw materials including cyclic carbonate to perform thermal decomposition reaction, regulating pressure by a vacuum control unit, vaporizing reaction products, collecting, and recovering unreacted raw materials.
In the invention, the cyclic carbonate is used as a reaction raw material, is heated and then decomposed into the epoxy compound and the carbon dioxide, and the reaction product can be separated from the raw material by adjusting the pressure, and the epoxy compound and the carbon dioxide can be easily separated; moreover, the reaction is simpler, the byproducts are less, and the yield of the epoxy compound is higher.
In a preferred embodiment of the present invention, the cyclic carbonate has a general structural formula:
wherein R is1And R2Independently any one of an alkyl group with H, C atoms of 1-10, an alcohol with 1-10 carbon atoms, an acid with 1-10 carbon atoms or an ester with 1-10 carbon atoms, for example, any one of 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10 carbon atoms.
Preferably, the reaction product is an epoxy compound having the general structural formula:
wherein R is1And R2Independently any one of an alkyl group having H, C atoms of 1-10, an alcohol having 1-10 carbon atoms, an acid having 1-10 carbon atoms, or an ester having 1-10 carbon atoms, for exampleThe number of C atoms may be any of 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10.
In the present invention, R in the structural formula of the raw material cyclic carbonate and the product epoxy compound1Same, R in the reaction raw materials1After radical determination, R in the reaction product1The same applies to R, consistent therewith2A group; wherein R is1、R2The selection of the species is that the alcohol, acid or ester is independently a group containing the corresponding functional group.
As a preferred technical scheme of the invention, the raw materials also comprise a solvent and a catalyst.
Preferably, the solvent comprises any one or a combination of at least two of alkane, alkane derivative, benzene derivative or ionic liquid; the alkane comprises straight-chain alkane and/or cycloalkane, the alkane derivative comprises halogenated alkane and the like, the benzene derivative comprises any one or combination of at least two of toluene, xylene, chlorobenzene, o-dichlorobenzene, p-dichlorobenzene, monochlorobiphenyl, diphenylmethane, dialkyl terephthalate or diethyl phthalate, and the ionic liquid comprises any one or combination of at least two of imidazole ionic liquid, pyridine ionic liquid or quaternary ammonium salt ionic liquid.
Preferably, the catalyst comprises an alkaline earth metal oxide and/or a transition metal oxide, wherein the alkaline earth metal oxide comprises magnesium oxide or the like; transition metal oxides include any one or a combination of at least two of titanium dioxide, chromium oxide, manganese dioxide, iron oxide, copper oxide, gold oxide, or lead oxide, with typical but non-limiting examples being: combinations of titanium dioxide and chromium oxide, iron oxide and copper oxide, titanium dioxide, manganese dioxide, and lead oxide, and the like.
Preferably, the support of the catalyst comprises any one of silica, alumina or molecular sieves, or a combination of at least two of these, typical but non-limiting examples being: combinations of silica and alumina, combinations of alumina and molecular sieves, combinations of silica, alumina or molecular sieves, and the like.
Preferably, the cyclic carbonate is present in an amount of 5 to 100 wt%, for example 5 wt%, 10 wt%, 20 wt%, 40 wt%, 50 wt%, 60 wt%, 80 wt% or 100 wt%, based on the weight of the raw material, but not limited to the recited values, and other values not recited within the range of the values are also applicable, preferably 20 to 90 wt%.
Preferably, the solvent is present in an amount of 0 to 95 wt%, for example 0 wt%, 10 wt%, 20 wt%, 40 wt%, 50 wt%, 60 wt%, 80 wt% or 95 wt%, based on the weight of the raw material, but not limited to the recited values, and other values not recited within the range of values are also applicable, preferably 20 to 60 wt%.
Preferably, the catalyst is present in an amount of 0 to 50 wt%, such as 0 wt%, 10 wt%, 20 wt%, 30 wt%, 40 wt% or 50 wt%, based on the weight of the feedstock, but not limited to the recited values, and other values not recited within this range are equally applicable, preferably 0 to 10 wt%.
In the invention, the raw materials of the cyclic carbonate and the solvent can be mixed and preheated in the premixing unit and then enter the reactor for reaction.
In a preferred embodiment of the present invention, the temperature of the thermal decomposition reaction is 50 to 350 ℃, for example, 50 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃ or 350 ℃, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable, and preferably 100 to 250 ℃.
Preferably, the thermal decomposition reaction is carried out in a reaction separation unit.
Generally, in the prior art, cyclic carbonate is prepared from an epoxy compound and carbon dioxide, in the application, the cyclic carbonate is used as a raw material to reversely prepare the epoxy compound, and meanwhile, the reaction temperature is not high and the reaction conditions are mild; if the temperature of the thermal decomposition reaction is higher, the cyclic carbonate can be quickly decomposed to generate a large amount of epoxy compounds which are difficult to quickly separate out, so that the epoxy compounds are polymerized, and the yield of the epoxy compounds is reduced; if the temperature of the thermal decomposition reaction is lower, the thermal decomposition rate of the cyclic carbonate is too low, the reaction efficiency of the reactor is rapidly reduced, the running flux is increased, and the difficulty of control operation is increased.
As the preferable technical scheme of the invention, the absolute pressure after the adjustment of the vacuum control unit is 1-105Pa, e.g. 1Pa, 10Pa, 100Pa, 500Pa, 1000Pa, 5000Pa, 10000Pa, 50000Pa or 10Pa5Pa, etc., but is not limited to the recited values, and other values not recited in the above range are also applicable, and preferably 200 to 105Pa。
As a preferred technical scheme of the invention, the reaction product is collected into a product collecting unit.
Preferably, the unreacted raw materials include a solvent, a catalyst and unreacted cyclic carbonate.
Preferably, the unreacted starting materials enter a recovery unit.
As a preferred technical solution of the present invention, the method comprises: adding cyclic carbonate, a solvent and a catalyst into a reaction separation unit, heating to 50-350 ℃ for thermal decomposition reaction, and adjusting the pressure to 1-10 by a vacuum control unit5Pa, the reaction product is vaporized and then collected into a product collecting unit, and the solvent, the catalyst and the unreacted cyclic carbonate enter a recovery unit.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method for preparing the epoxy compound by using the cyclic carbonate as the raw material has high efficiency, the conversion of the cyclic carbonate can reach more than 92.8 percent and can reach more than 99 percent at most, and the selectivity of the epoxy compound is high and can reach more than 99 percent;
(2) the device integrates the reaction and separation processes into the same unit, can simplify the process flow, and is suitable for synthesis of various epoxy compounds;
(3) the method can directly synthesize the epoxy compound, and has mild reaction conditions and lower risk coefficient.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing an epoxy compound by a batch reaction according to example 1 of the present invention;
FIG. 2 is a schematic structural view of an apparatus for preparing an epoxy compound by a batch reaction provided in example 6 of the present invention;
FIG. 3 is a schematic view of the structure of an apparatus for preparing an epoxy compound by a batch reaction provided in example 11 of the present invention;
the system comprises a reactor 1, a reactor 2, a separator 3, a product collecting unit, a vacuum control unit 4, a recovery unit 5, a tower reactor 6, a premixing tank 7, a tubular reactor 8 and a flash tank 9.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the following embodiments are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The invention provides a device and a method for preparing an epoxy compound by a batch reaction, the device comprises a reaction separation unit, a product collection unit 3, a vacuum control unit 4 and a recovery unit 5, an upper outlet of the reaction separation unit is connected with the product collection unit 3, the product collection unit 3 is connected with the vacuum control unit 4, and a lower outlet of the reaction separation unit is connected with the recovery unit 5.
The method comprises the following steps: heating raw materials including cyclic carbonate to perform thermal decomposition reaction, regulating pressure by a vacuum control unit 4, vaporizing reaction products, collecting, and recovering unreacted raw materials.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a device and a method for preparing an epoxy compound by a batch reaction, wherein the device has a schematic structural diagram shown in fig. 1 and comprises a reaction separation unit, a product collection unit 3, a vacuum control unit 4 and a recovery unit 5, an upper outlet of the reaction separation unit is connected with the product collection unit 3, the product collection unit 3 is connected with the vacuum control unit 4, and a lower outlet of the reaction separation unit is connected with the recovery unit 5; the reaction separation unit includes a tank reactor 1 and a separator 2.
The method is carried out in the device of the embodiment and comprises the following steps:
adding the cyclic carbonate, the solvent and the catalyst into the kettle-type reactor 1, heating to a reaction temperature, continuously thermally decomposing the epoxy compound, continuously vaporizing a reaction product by adjusting the vacuum degree of the vacuum control unit 4, and collecting the product to the product collection unit 3. And when the product collection unit 3 cannot collect any liquid product, stopping heating, discharging the reaction residue to the recovery unit 5, respectively analyzing and detecting the materials in the product collection unit 3 and the recovery unit 5, and comprehensively obtaining the conversion rate of the cyclic carbonate, the yield of the epoxy compound and the selectivity of the epoxy compound.
Examples 2 to 5:
the above examples all provide an apparatus and a method for preparing an epoxy compound by a batch reaction, the structure of the apparatus is as in example 1, and the method is as in example 1.
The reaction feed parameters in examples 1-5 were summarized and the results are shown in Table 1, and the reaction operating parameters were summarized and the results are shown in Table 2; the products obtained in examples 1 to 5 were analyzed and measured, and the conversion of the raw material, the yield of the product and the selectivity were calculated, and the results are shown in Table 3.
TABLE 1 summary of reaction feed parameters described in examples 1-5
TABLE 2 summary of operating parameters of the reactions described in examples 1-5
TABLE 3 analytical test results for the products obtained in examples 1 to 5
Example 6:
the embodiment provides a device and a method for preparing an epoxy compound by a batch reaction, wherein the device has a schematic structural diagram shown in fig. 2 and comprises a reaction separation unit, a product collection unit 3, a vacuum control unit 4 and a recovery unit 5, an upper outlet of the reaction separation unit is connected with the product collection unit 3, the product collection unit 3 is connected with the vacuum control unit 4, and a lower outlet of the reaction separation unit is connected with the recovery unit 5; the reaction separation unit comprises a tower reactor 6, and the tower reactor 6 is a packed tower.
The method is carried out in the device of the embodiment and comprises the following steps:
the cyclic carbonate, the solvent and the catalyst are added into a tower kettle of a tower reactor 6 at one time, the mixture is heated to the reaction temperature, the epoxy compound is continuously thermally decomposed, the reaction product is continuously vaporized by adjusting the vacuum degree of a vacuum control unit 4, reboiling steam is provided for the tower reactor, and the rectified product is extracted from the tower and enters a product collection unit 3. And when the product collection unit 3 cannot collect any liquid product, stopping heating, discharging the reaction residue to the recovery unit 5, respectively analyzing and detecting the materials in the product collection unit 3 and the recovery unit 5, and comprehensively obtaining the conversion rate of the cyclic carbonate, the yield of the epoxy compound and the selectivity of the epoxy compound.
Examples 7 to 10:
the above examples all provide an apparatus and a method for preparing an epoxy compound by a batch reaction, the structure of the apparatus is as in example 6, and the method is as in example 6.
The reaction feed parameters in examples 6-10 were summarized and the results are shown in Table 4, and the reaction operating parameters were summarized and the results are shown in Table 5; the products obtained in examples 6 to 10 were analyzed and examined, and the conversion of the raw material, the yield of the product and the selectivity were calculated, and the results are shown in Table 6.
TABLE 4 summary of reaction feed parameters described in examples 6-10
TABLE 5 summary of the operating parameters of the reactions described in examples 6-10
TABLE 6 analysis and examination of the products obtained in examples 6 to 10
Example 11:
the embodiment provides a device and a method for preparing an epoxy compound by a batch reaction, wherein the device has a schematic structural diagram shown in fig. 3, and comprises a reaction separation unit, a product collection unit 3, a vacuum control unit 4 and a recovery unit 5, an upper outlet of the reaction separation unit is connected with the product collection unit 3, the product collection unit 3 is connected with the vacuum control unit 4, and a lower outlet of the reaction separation unit is connected with the recovery unit 5; the reaction separation unit comprises a tubular reactor 8 and a flash tank 9;
the device also comprises a premixing tank 7, wherein the premixing tank 7 is connected with the tubular reactor 8 through a pump.
The method is carried out in the device of the embodiment and comprises the following steps:
adding the cyclic carbonate and the solvent into a premixing tank 7, heating to 50 ℃ until the cyclic carbonate and the solvent are completely dissolved, then starting a pump, conveying the cyclic carbonate solution to a tubular reactor 8, heating to the reaction temperature, passing through a catalyst bed layer, thermally decomposing the cyclic carbonate into an epoxy compound, finally injecting the epoxy compound into a flash tank 9, adjusting the vacuum degree of the flash tank 9 through a vacuum control unit 4, and vaporizing the epoxy compound after entering to separate the epoxy compound from the solvent. The vaporized epoxy compound enters a product collecting unit 3, the cyclic carbonate and the solvent which are not thermally decomposed are discharged to a recovery unit 5, and the materials in the product collecting unit 3 and the materials in the recovery unit 5 are analyzed and detected respectively, so that the conversion rate of the cyclic carbonate, the yield of the epoxy compound and the selectivity of the epoxy compound are comprehensively obtained.
Examples 12 to 13:
the above examples all provide an apparatus and a method for preparing an epoxy compound by a batch reaction, the structure of the apparatus is as in example 11, and the method is as in example 11.
The reaction feed parameters in examples 11-13 were summarized and the results are shown in Table 7, and the reaction operating parameters were summarized and the results are shown in Table 8; the products obtained in examples 11 to 13 were analyzed and measured, and the conversion of the raw material, the yield of the product and the selectivity were calculated, and the results are shown in Table 9.
TABLE 7 summary of reaction feed parameters described in examples 11-13
TABLE 8 summary of the operating parameters of the reactions described in examples 11-13
TABLE 9 analytical test results for the products obtained in examples 11 to 13
The device and the method are adopted to prepare the epoxy compound, and as can be seen from table 3, when the kettle type reactor is adopted in the examples 1-5, the conversion rate of the cyclic carbonate can reach more than 94.8 percent, the highest conversion rate can reach 99.6 percent, and the selectivity of the product is more than 99.5 percent; as can be seen from Table 6, in examples 6 to 10, when the column reactor was used, the conversion of the cyclic carbonate was 95.8% or more, and the highest conversion was 99.1%, and the product selectivity was 99.4 or more; as can be seen from Table 9, in examples 11 to 13, tubular reactors were used, which were of different reactor types, so that the conversion of cyclic carbonate was slightly lower but was also higher than 92.8%, but the product selectivities were all higher than 99.9%; the above results are slightly different, depending on the type of reactor used, and can be selected according to the actual needs, expanding the range of applications of the device; the method has high production efficiency in the process flow section and is suitable for synthesizing various epoxy compounds.
The applicant states that the present invention is illustrated by the above examples to describe the detailed apparatus and process of the present invention, but the present invention is not limited to the above apparatus and process, i.e. it is not meant to imply that the present invention must be implemented by the above apparatus and process. It will be apparent to those skilled in the art that any modifications to the present invention, equivalent alterations to the devices and processes of the present invention, additions of auxiliary devices or components, and selection of particular means, are within the scope and disclosure of the present invention.
Claims (28)
1. The device for preparing the epoxy compound by the batch reaction is characterized by comprising a reaction separation unit, a product collection unit, a vacuum control unit and a recovery unit, wherein an upper outlet of the reaction separation unit is connected with the product collection unit, the product collection unit is connected with the vacuum control unit, and a lower outlet of the reaction separation unit is connected with the recovery unit;
the reaction separation unit comprises a reactor and a separator, the reactor and the separator are in the same device, and the catalyst for reaction comprises alkaline earth metal oxide and/or transition metal oxide.
2. The apparatus of claim 1, wherein the reactive separation unit comprises any one of a tank reactor, a membrane reactor, a column reactor, or a tubular reactor, or a combination of at least two thereof.
3. The apparatus of claim 2, wherein the tank reactor comprises any one of or a combination of at least two of an internal circulation reaction tank, an internal gas circulation reaction tank, an internal catalyst holder reaction tank, an internal baffle reaction tank and an external forced circulation system reaction tank.
4. The apparatus of claim 2 wherein the membrane reactor comprises any one or a combination of at least two of a falling film reactor, a rising film reactor or a wiped film reactor.
5. The apparatus of claim 2, wherein the column reactor comprises any one of a packed column, a float valve column, or a sieve plate column, or a combination of at least two of them.
6. The apparatus of claim 2, wherein the tubular reactor comprises any one of a single tubular reactor, a multi-tubular reactor, a forced plug flow tubular reactor, or a forced back-mixed tubular reactor, or a combination of at least two thereof.
7. A method for preparing an epoxy compound using the apparatus of any one of claims 1-6, the method comprising: heating raw materials including cyclic carbonate to perform thermal decomposition reaction, regulating pressure by a vacuum control unit, vaporizing reaction products, collecting, and recovering unreacted raw materials.
8. The method of claim 7, wherein the cyclic carbonate has the general structural formula:
wherein R is1And R2Independently any one of an alkyl group with H, C atomic number of 1-10, an alcohol with 1-10 atomic number of C, an acid with 1-10 atomic number of C or an ester with 1-10 atomic number of C.
9. The method of claim 7, wherein the reaction product is an epoxy compound having the general structural formula:
wherein R is1And R2Independently any one of an alkyl group with H, C atomic number of 1-10, an alcohol with 1-10 atomic number of C, an acid with 1-10 atomic number of C or an ester with 1-10 atomic number of C.
10. The method of claim 7, wherein the feedstock further comprises a solvent and a catalyst.
11. The method of claim 10, wherein the solvent comprises any one of or a combination of at least two of an alkane, an alkane derivative, benzene, a benzene derivative, or an ionic liquid.
12. The method of claim 10, wherein the catalyst comprises an alkaline earth metal oxide and/or a transition metal oxide.
13. The process of claim 10, wherein the support of the catalyst comprises any one of silica, alumina, or molecular sieves, or a combination of at least two thereof.
14. The method according to claim 10, wherein the cyclic carbonate accounts for 5 to 100 wt% of the raw material.
15. The method according to claim 14, wherein the cyclic carbonate accounts for 20 to 90 wt% of the raw material.
16. The method according to claim 10, wherein the solvent accounts for 0-95 wt% of the raw materials.
17. The method according to claim 16, wherein the solvent accounts for 20-60 wt% of the raw materials.
18. The method according to claim 10, wherein the catalyst accounts for 0-50 wt% of the raw material.
19. The method of claim 18, wherein the catalyst is present in an amount of 0 to 10 wt.% based on the weight of the feedstock.
20. The method according to claim 7, wherein the temperature of the thermal decomposition reaction is 50 to 350 ℃.
21. The method according to claim 20, wherein the temperature of the thermal decomposition reaction is 100 to 250 ℃.
22. The method of claim 7, wherein the thermal decomposition reaction is performed in a reaction separation unit.
23. The method according to claim 7, wherein the absolute pressure after the adjustment by the vacuum control unit is 1-105Pa。
24. The method according to claim 23, wherein the vacuum control unit adjusts the absolute pressure to 200-10%5Pa。
25. The method of claim 7, wherein the reaction product is collected in a product collection unit.
26. The method of claim 7, wherein the unreacted starting materials comprise a solvent, a catalyst, and unreacted cyclic carbonate.
27. The method of claim 7, wherein the unreacted feedstock enters a recovery unit.
28. The method of claim 7, wherein the method comprises: adding cyclic carbonate, a solvent and a catalyst into a reaction separation unit, heating to 50-350 ℃, and adjusting the pressure to 1-10 ℃ through a vacuum control unit5Pa, the reaction product is vaporized and then collected into a product collecting unit, and the solvent, the catalyst and the unreacted cyclic carbonate enter a recovery unit.
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