CN110156724A - A kind of intermittent reaction prepares the device and method of epoxide - Google Patents
A kind of intermittent reaction prepares the device and method of epoxide Download PDFInfo
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- CN110156724A CN110156724A CN201910549058.4A CN201910549058A CN110156724A CN 110156724 A CN110156724 A CN 110156724A CN 201910549058 A CN201910549058 A CN 201910549058A CN 110156724 A CN110156724 A CN 110156724A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- 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
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
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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
- C07D303/14—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by free hydroxyl radicals
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention provides the device and methods that a kind of intermittent reaction prepares epoxide, described device includes Reaction Separation unit, collection of products unit, vacuum control unit and recovery unit, the upper outlet of the Reaction Separation unit is connected with collection of products unit, the collection of products unit is connected with vacuum control unit, and the lower part outlet of the Reaction Separation unit is connected with recovery unit.Device of the present invention will react and separation process is integrated into same unit, and reactor plays an important role to reaction efficiency with separator combination collocation, and suitable for the synthesis of various epoxides, condition is milder, and danger coefficient is small；The method is high-efficient, while the yield of epoxide and selectivity are high.
Description
Technical field
The invention belongs to technical field of organic synthesis, it is related to device and side that a kind of intermittent reaction prepares epoxide
Method.
Background technique
Epoxide is a kind of compound with ternary cyclic ether structure, wherein simplest compound is epoxy second
Alkane.The same with cyclopropane, the ring strain of epoxide is very big, and tension can be 114.1kJ/mol, has stronger chemistry
Activity can be reacted with a variety of compounds.The representative species of epoxide have ethylene oxide, propylene oxide, 1,2- ring
Oxygen butane, 2,3- epoxy butane, 1,2- epoxypentane, 2,3- epoxypentane etc..The huge market demand of epoxide is one
The important Organic chemical products of class, however, there was only the technology of preparing of the simple epoxide such as ethylene oxide, propylene oxide at present
More mature, there are still many difficulties for the epoxide of other macromolecules.
Currently, the production line of epoxide mainly has direct oxidation method and indirect oxidation method.CN 104650008A is public
A kind of technique and system for preparing propylene oxide by oxygen, hydrogen direct oxidation propylene has been opened, propylene, circulation propylene, higher boiling have been had
Machine sulfide is added to the in the mixed solvent of methanol and hydrazine hydrate, is passed through hydrogen and oxygen, generates propylene oxide crude product, thick to produce
Product successively pass through crude tower, propylene stripper, and remaining propylene oxide mixed liquor enters the extraction containing isopropylbenzene and alkaline solution
Purification column is taken, further extracting rectifying obtains the product propylene of high-purity.CN 108947938A, which is disclosed, a kind of prepares ring
Logistics comprising ethane is first placed under the conditions of oxidative dehydrogenation to prepare ethylene, then will described include ethylene by the method for Ethylene Oxide
Logistics with unconverted ethane is placed in oxidizing condition and gets off to prepare ethylene oxide, and generating includes ethylene oxide, unconverted second
The logistics of alkene and ethane, then separating ethylene oxide is recycled from the logistics.However, oxidizing process is prepared needed for epoxide at present
Condition is more harsh, is easy explosion, does not conform to symbol safety in production and requires, therefore, researcher, which also has, continually develops new epoxy compound
The preparation method of object.
Thermal decomposition method is to prepare inorganic material a kind of commonly method, in organic matter using less, according to epoxidation
The generable reaction of object is closed, the new method that epoxide is a kind of worth research is reversely prepared by its product, to solve
Complex steps, the problem that separation is difficult, safety is low in existing method.
Summary of the invention
The prior art there are aiming at the problem that, the purpose of the present invention is to provide a kind of intermittent reactions to prepare epoxy compound
The device and method of object, the present invention prepare epoxide using epoxy carbonate as raw material, using decomposition method, by reaction and separation
It is carried out in set of procedures to Reaction Separation unit, product yield not only can be improved, but also can simplification of flowsheet；The method is suitable for
A variety of epoxides, reaction condition are mild.
To achieve this purpose, the present invention adopts the following technical scheme:
On the one hand, the present invention provides the device that a kind of intermittent reaction prepares epoxide, described device includes reaction
Separative unit, collection of products unit, vacuum control unit and recovery unit, the upper outlet and product of the Reaction Separation unit
Collector unit be connected, the collection of products unit is connected with vacuum control unit, the lower part outlet of the Reaction Separation unit and
Recovery unit is connected.
In the present invention, described device is used to prepare epoxide, each in selection device according to reactant and reaction type
Reaction, separation are integrated into a unit by unit and its connection relationship, and reaction product in time and reactants separate, is conducive to
The positive of reaction carries out, and improves the conversion ratio of reactant, while can reduce device quantity, reduces cost.
It is used as currently preferred technical solution below, but not as the limitation of technical solution provided by the invention, passes through
Following technical scheme can preferably reach and realize technical purpose and beneficial effect of the invention.
As currently preferred technical solution, the Reaction Separation unit includes reactor and separator, the reaction
Device and separator in the same device or belong to distinct device.
Preferably, the Reaction Separation unit includes tank reactor, membrane reactor, tower reactor or tubular reactor
In any one or at least two combination, the combination is typical but non-limiting example has: tank reactor and membrane reactor
Combination, the combination of membrane reactor and tower reactor, tank reactor, tower reactor and combination of tubular reactor etc..
In the present invention, Reaction Separation unit is formed by reactor and separator set, and the two can in the same device, this
When only react and separate two kinds operation differentiations, in tank reactor, on reboiler, tower reactor or a certain column plate, rise
Steam be reaction product；The two can not also in the same device, such as the combination of tubular reactor and thin film evaporator,
Thin film evaporator can separate reaction product with reactant.The matched combined of reactor and separator, and it is selected anti-
It answers device type related, the height of reaction efficiency is had a major impact.
As currently preferred technical solution, the tank reactor includes that built-in circulation reaction kettle, built-in gas follow
Ring reaction kettle, built-in catalyst fixator reaction kettle, internal baffle reaction kettle or external forced circulation system reaction kettle in appoint
It anticipates a kind of or at least two combinations, the combination typical case but non-limiting example has: built-in circulation reaction kettle and built-in gas
The combination of circular response kettle, the combination of built-in catalyst fixator reaction kettle and internal baffle reaction kettle, built-in circulation reaction kettle,
The combination etc. of built-in catalyst fixator reaction kettle and the reaction kettle of external forced circulation system.
Wherein, the external forced circulation system of reaction kettle includes the function such as external heat exchanger, external pipe type reactor, rectifying column
It can property component.
Preferably, the membrane reactor include falling film reactor, rise membrane reactor or scrape any one in membrane reactor or
At least two combination, the combination is typical but non-limiting example has: falling film reactor and the combination for rising membrane reactor rise film
Reactor and the combination for scraping membrane reactor, falling film reactor rise membrane reactor and scrape the combination of membrane reactor etc..
Preferably, the tower reactor includes any one in packed tower, valve tower or sieve-plate tower or at least two
Combination, the combination is typical but non-limiting example has: the combination of the combination of packed tower and valve tower, valve tower and sieve-plate tower,
Packed tower, valve tower and combination of sieve-plate tower etc..
Preferably, the tubular reactor includes single hose reactor, multi-tubular reactor, forces plug flow pipe reaction
Device or the combination for forcing any one in back-mixing tubular reactor or at least two, the combination typical case but non-limiting example
Have: the combination of single hose reactor and multi-tubular reactor forces plug flow reactor and forces back-mixing tubular reactor
Combination, single hose reactor, multi-tubular reactor and the combination etc. for forcing plug flow reactor.
In the present invention, described device further includes premixing cell, and the premixing cell is connected with Reaction Separation unit.
On the other hand, the present invention provides a kind of method for preparing epoxide using above-mentioned apparatus, the method packets
It includes: will include the raw material heating of cyclic carbonate, pyrolysis occurs, pressure is adjusted by vacuum control unit, reaction produces
It is collected after object vaporization, unreacting material is recycled.
In the present invention, cyclic carbonate is decomposed into epoxide and carbon dioxide after heat temperature raising as reaction raw materials,
By adjusting pressure, reaction product can be separated with raw material, and epoxide and carbon dioxide also can be easily separated；And institute
It states and reacts relatively simple, by-product is few, and the yield of epoxide is higher.
As currently preferred technical solution, the general structure of the cyclic carbonate are as follows:
Wherein, R1And R2Independently being the alkyl that H, C atomicity are 1~10, the alcohols that C atomicity is 1~10, C atomicity is 1~10
Acids or C atomicity be 1~10 esters in any one, such as C atomicity can be 1,2,3,4,5,6,7,8,9 or 10
In any one.
Preferably, the reaction product is epoxide, general structure are as follows:Wherein R1And R2
It independently is the acids or C original that the alkyl that H, C atomicity are 1~10, the alcohols that C atomicity is 1~10, C atomicity are 1~10
Any one in the esters that subnumber is 1~10, such as C atomicity can be any one in 1,2,3,4,5,6,7,8,9 or 10.
R in the present invention, in the structural formula of raw material cyclic carbonate and product epoxide1It is identical, in reaction raw materials
R1After group determines, the R in reaction product1Then consistent with its, above-mentioned statement is equally applicable to R2Group；Wherein R1、R2Type
Selection in alcohols, acids or esters independently be the group containing corresponding functional group.
As currently preferred technical solution, the raw material further includes solvent and catalyst.
Preferably, the solvent include any one in alkane, alkane derivatives, benzene, benzene derivative or ionic liquid or
At least two combination；Wherein, alkane includes linear paraffin and/or cycloalkane, and alkane derivatives include halogenated alkane etc., and benzene spreads out
Biology includes toluene, dimethylbenzene, chlorobenzene, o-dichlorohenzene, paracide, a chlordiphenyl, diphenyl methane, terephthalic acid (TPA) dioxane
Any one in base ester or diethyl phthalate or at least two combination, ionic liquid include glyoxaline ion liquid,
Any one in pyridine ionic liquid or ion liquid of quaternaries or at least two combination.
Preferably, the catalyst includes alkaline earth oxide and/or transition metal oxide, wherein alkaline-earth metal oxygen
Compound includes magnesia etc.；Transition metal oxide includes titanium dioxide, chrome green, manganese dioxide, iron oxide, oxidation
Any one in copper, gold oxide or lead oxide or at least two combination, the combination is typical but non-limiting example has: dioxy
Change the combination of titanium and chrome green, the combination of iron oxide and copper oxide, the combination of titanium dioxide, manganese dioxide and lead oxide
Deng.
Preferably, the carrier of the catalyst includes any one in silica, aluminium oxide or molecular sieve or at least two
The combination of kind, the combination is typical but non-limiting example has: the combination of silica and aluminium oxide, aluminium oxide and molecular sieve
Combination, silica, aluminium oxide or combination of molecular sieve etc..
Preferably, the cyclic carbonate accounts for the mass fraction of raw material as 5~100wt%, such as 5wt%, 10wt%,
20wt%, 40wt%, 50wt%, 60wt%, 80wt% or 100wt% etc., it is not limited to cited numerical value, the numerical value
Other unlisted numerical value are equally applicable in range, preferably 20~90wt%.
Preferably, the solvent account for raw material mass fraction be 0~95wt%, such as 0wt%, 10wt%, 20wt%,
40wt%, 50wt%, 60wt%, 80wt% or 95wt% etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable, preferably 20~60wt%.
Preferably, the catalyst account for raw material mass fraction be 0~50wt%, such as 0wt%, 10wt%, 20wt%,
30wt%, 40wt% or 50wt% etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range
It is equally applicable, preferably 0~10wt%.
In the present invention, raw material cyclic carbonate and solvent can first mix preheating in premixing cell, subsequently into reaction
Device reacts.
As currently preferred technical solution, the temperature of the pyrolysis is 50~350 DEG C, such as 50 DEG C, 100
DEG C, 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C or 350 DEG C etc., it is not limited to cited numerical value, in the numberical range other
Unlisted numerical value is equally applicable, and preferably 100~250 DEG C.
Preferably, the pyrolysis carries out in Reaction Separation unit.
In general, be that cyclic carbonate is prepared by epoxide and carbon dioxide in the prior art, and the application
In using cyclic carbonate as raw material, reversely prepare epoxide, simultaneous reactions required temperature is not high, and condition is more mild；If
The temperature drift of pyrolysis can make cyclic carbonate fast decoupled, generate a large amount of epoxide, it is difficult to quickly divide
It separates out, causes epoxide self-polymerization, reduce the yield of epoxide；If the temperature of pyrolysis is relatively low,
It will cause cyclic carbonate rhermal decomposition rate is too small, reactor reaction efficiency is quickly reduced, and increases operating flux, increases control
The difficulty of operation.
As currently preferred technical solution, absolute pressure is 1~10 after the vacuum control unit is adjusted5Pa, example
Such as 1Pa, 10Pa, 100Pa, 500Pa, 1000Pa, 5000Pa, 10000Pa, 50000Pa or 105Pa etc., it is not limited to institute
The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable, and preferably 200~105Pa。
As currently preferred technical solution, the reaction product is collected into collection of products unit.
Preferably, the unreacting material includes solvent, catalyst and unreacted cyclic carbonate.
Preferably, the unreacting material enters recovery unit.
As currently preferred technical solution, which comprises cyclic carbonate, solvent and catalyst are added anti-
Answer and be heated to 50~350 DEG C after separative unit, pyrolysis occurs, by vacuum control unit adjust pressure to 1~
105Pa is collected after reaction product vaporization into collection of products unit, and solvent, catalyst and unreacted cyclic carbonate enter
Recovery unit.
Compared with prior art, the invention has the following advantages:
(1) present invention prepares epoxide by raw material of cyclic carbonate, and the method is high-efficient, cyclic carbonate
Conversion is up to 92.8% or more, up to 99% or more, and epoxide selectivity is high, up to 99% or more；
(2) device of the present invention by react and separation process be integrated into same unit, can simplification of flowsheet, fit
Synthesis for various epoxides；
(3) the method for the invention can direct synthesizing epoxy compound, reaction condition is mild, and danger coefficient is relatively low.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram that the intermittent reaction that the embodiment of the present invention 1 provides prepares epoxide；
Fig. 2 is the apparatus structure schematic diagram that the intermittent reaction that the embodiment of the present invention 6 provides prepares epoxide；
Fig. 3 is the apparatus structure schematic diagram that the intermittent reaction that the embodiment of the present invention 11 provides prepares epoxide；
Wherein, 1- tank reactor, 2- separator, 3- collection of products unit, 4- vacuum control unit, 5- recovery unit,
6- tower reactor, 7- premixing tank, 8- tubular reactor, 9- flash tank.
Specific embodiment
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, below further specifically to the present invention
Bright but following embodiment is only simple example of the invention, does not represent or limit the scope of the present invention, this hair
Bright protection scope is subject to claims.
Specific embodiment of the invention part provides the device and method that a kind of intermittent reaction prepares epoxide, institute
Stating device includes Reaction Separation unit, collection of products unit 3, vacuum control unit 4 and recovery unit 5, the Reaction Separation list
The upper outlet of member is connected with collection of products unit 3, and the collection of products unit 3 is connected with vacuum control unit 4, the reaction
The lower part outlet of separative unit is connected with recovery unit 5.
The described method includes: the raw material including cyclic carbonate is heated, pyrolysis occurs, passes through vacuum control list
Member 4 adjusts pressure, collects after reaction product vaporization, unreacting material is recycled.
The following are typical but non-limiting embodiments of the invention:
Embodiment 1:
The device and method that a kind of intermittent reaction prepares epoxide is present embodiments provided, the structure of described device is shown
It is intended to as shown in Figure 1, include Reaction Separation unit, collection of products unit 3, vacuum control unit 4 and recovery unit 5, it is described anti-
The upper outlet of separative unit is answered to be connected with collection of products unit 3, the collection of products unit 3 is connected with vacuum control unit 4,
The lower part outlet of the Reaction Separation unit is connected with recovery unit 5；The Reaction Separation unit includes tank reactor 1 and divides
From device 2.
The method carries out in the present embodiment described device, comprising the following steps:
Cyclic carbonate, solvent and catalyst are added in tank reactor 1, reaction temperature, epoxide are heated to
Lasting thermal decomposition realizes that reaction product constantly vaporizes, collection of products to product by adjusting the vacuum degree of vacuum control unit 4
Collector unit 3.After collection of products unit 3 is collected less than any product liquid, stops heating, reaction residue is discharged to recycling
Unit 5, carries out analysis detection to the material in product collector unit 3 and recovery unit 5 respectively, and the comprehensive cyclic carbonate that obtains turns
The selectivity of rate, the yield of epoxide and epoxide.
Embodiment 2-5:
Above-described embodiment is each provided with the device and method that a kind of intermittent reaction prepares epoxide, the knot of described device
Structure is referring to the device in embodiment 1, and the method is referring to the method in embodiment 1.
Reaction feed parameter in embodiment 1-5 is summarized, the results are shown in Table 1, and operation parameter is carried out
Summarize, the results are shown in Table 2；Product obtained in embodiment 1-5 is subjected to analysis detection, calculates conversion ratio, the product of raw material
Yield and selectivity, the results are shown in Table 3.
Reaction feed parameter described in 1 embodiment 1-5 of table summarizes
Operation parameter described in 2 embodiment 1-5 of table summarizes
The analysis detection result of products therefrom in 3 embodiment 1-5 of table
Embodiment 6:
Present embodiments provide the device and method that a kind of intermittent reaction prepares epoxide, described device structural representation
Figure is as shown in Fig. 2, include Reaction Separation unit, collection of products unit 3, vacuum control unit 4 and recovery unit 5, the reaction
The upper outlet of separative unit is connected with collection of products unit 3, and the collection of products unit 3 is connected with vacuum control unit 4, institute
The lower part outlet for stating Reaction Separation unit is connected with recovery unit 5；The Reaction Separation unit includes tower reactor 6, described
Tower reactor 6 is packed tower.
The method carries out in the present embodiment described device, comprising the following steps:
Cyclic carbonate, solvent and catalyst are added at one time in the tower reactor of tower reactor 6, are heated to reaction temperature
Degree, epoxide persistently thermally decompose, and by adjusting the vacuum degree of vacuum control unit 4, realize that reaction product constantly vaporizes, are
Vapour is boiled in tower reactor offer again, and the product after rectifying is produced from tower, into collection of products unit 3.When collection of products list
After member 3 is collected less than any product liquid, stop heating, reaction residue is discharged to recovery unit 5, product is collected respectively single
Material in member 3 and recovery unit 5 carries out analysis detection, and synthesis obtains the yield of cyclic carbonate ester conversion rate, epoxide
With the selectivity of epoxide.
Embodiment 7-10:
Above-described embodiment is each provided with the device and method that a kind of intermittent reaction prepares epoxide, the knot of described device
Structure is referring to the device in embodiment 6, and the method is referring to the method in embodiment 6.
Reaction feed parameter in embodiment 6-10 is summarized, the results are shown in Table 4, and operation parameter is carried out
Summarize, the results are shown in Table 5；Product obtained in embodiment 6-10 is subjected to analysis detection, calculates conversion ratio, the product of raw material
Yield and selectivity, the results are shown in Table 6.
Reaction feed parameter described in 4 embodiment 6-10 of table summarizes
Operation parameter described in 5 embodiment 6-10 of table summarizes
The analysis detection result of products therefrom in 6 embodiment 6-10 of table
Embodiment 11:
Present embodiments provide the device and method that a kind of intermittent reaction prepares epoxide, described device structural representation
Figure is as shown in figure 3, include Reaction Separation unit, collection of products unit 3, vacuum control unit 4 and recovery unit 5, the reaction
The upper outlet of separative unit is connected with collection of products unit 3, and the collection of products unit 3 is connected with vacuum control unit 4, institute
The lower part outlet for stating Reaction Separation unit is connected with recovery unit 5；The Reaction Separation unit includes tubular reactor 8 and flash distillation
Tank 9；
Described device further includes premixing tank 7, and the premixing tank 7 is connected by pump with tubular reactor 8.
The method carries out in the present embodiment described device, comprising the following steps:
Cyclic carbonate, solvent are added in premixing tank 7, and are heated to 50 DEG C, until all dissolutions, then open pump,
Cyclic carbonate ester solution is delivered to tubular reactor 8, is heated to reaction temperature, passes through catalyst bed, cyclic carbonate heat
Epoxide is resolved into, flash tank 9 is finally injected into, flash tank 9 has passed through vacuum control unit 4 and adjusted vacuum degree, ring
Oxygen compound vaporizes after entering, and is separated with solvent.Epoxide after vaporization enters product collector unit 3, not heat point
The cyclic carbonate and solvent of solution are then discharged to recovery unit 5, respectively to the material in product collector unit 3 and recovery unit 5
Analysis detection is carried out, synthesis obtains the selectivity of cyclic carbonate ester conversion rate, the yield of epoxide and epoxide.
Embodiment 12-13:
Above-described embodiment is each provided with the device and method that a kind of intermittent reaction prepares epoxide, the knot of described device
Structure is referring to the device in embodiment 11, and the method is referring to the method in embodiment 11.
Reaction feed parameter in embodiment 11-13 is summarized, the results are shown in Table 7, by operation parameter into
Row summarizes, and the results are shown in Table 8；By product obtained in embodiment 11-13 carry out analysis detection, calculate raw material conversion ratio,
The yield and selectivity of product, the results are shown in Table 9.
Reaction feed parameter described in 7 embodiment 11-13 of table summarizes
Operation parameter described in 8 embodiment 11-13 of table summarizes
The analysis detection result of products therefrom in 9 embodiment 11-13 of table
The present invention carries out the preparation of epoxide using described device and method, and as shown in Table 3, embodiment 1-5 is used
When tank reactor, up to 94.8% or more, up to 99.6%, the selectivity of product exists cyclic carbonate ester conversion rate
99.5% or more；As shown in Table 6, when embodiment 6-10 uses tower reactor, cyclic carbonate ester conversion rate is up to 95.8%
More than, up to 99.1%, the selectivity of product reaches 99.4 or more at this time；As shown in Table 9, it is adopted in embodiment 11-13
With tubular reactor, type of reactor is different, so that cyclic carbonate ester conversion rate is slightly lower, but also reaches 92.8% or more, but
Selectivity of product is up to 99.9% or more；The above results are slightly different, related with reactor used type, can be according to reality
Border needs to extend the application range of described device to select；The method process flow section, high production efficiency are suitable for each
The synthesis of kind epoxide.
The Applicant declares that the present invention is explained by the above embodiments detailed device and process of the invention, but this
Invention is not limited to above-mentioned apparatus and method, that is, does not mean that the present invention must rely on above-mentioned apparatus and method and could implement.
It should be clear to those skilled in the art, any improvement in the present invention, replaces to apparatus of the present invention and the equivalent of technique
It changes, auxiliary device or the addition and the selection of concrete mode of ingredient etc., all falls within protection scope of the present invention and the open scope
Within.
Claims (10)
1. the device that a kind of intermittent reaction prepares epoxide, which is characterized in that described device includes Reaction Separation unit, produces
Object collector unit, vacuum control unit and recovery unit, upper outlet and the collection of products unit phase of the Reaction Separation unit
Even, the collection of products unit is connected with vacuum control unit, lower part outlet and the recovery unit phase of the Reaction Separation unit
Even.
2. the apparatus according to claim 1, which is characterized in that the Reaction Separation unit includes reactor and separator,
The reactor and separator in the same device or belong to distinct device；
Preferably, the Reaction Separation unit includes appointing in tank reactor, membrane reactor, tower reactor or tubular reactor
It anticipates a kind of or at least two combinations.
3. the apparatus of claim 2, which is characterized in that the tank reactor includes built-in circulation reaction kettle, interior
Set the anti-of gas circular response kettle, built-in catalyst fixator reaction kettle, internal baffle reaction kettle or external forced circulation system
Answer the combination of any one in kettle or at least two；
Preferably, the membrane reactor includes falling film reactor, rises membrane reactor or scrape any one in membrane reactor or at least
Two kinds of combination；
Preferably, the tower reactor includes the combination of any one in packed tower, valve tower or sieve-plate tower or at least two；
Preferably, the tubular reactor include single hose reactor, multi-tubular reactor, force plug flow reactor or
Force the combination of any one in back-mixing tubular reactor or at least two.
4. a kind of method for preparing epoxide using any one of claim 1-3 described device, which is characterized in that the side
Method includes: to heat the raw material including cyclic carbonate, and pyrolysis occurs, and adjusts pressure by vacuum control unit, instead
It is collected after answering product to vaporize, unreacting material is recycled.
5. according to the method described in claim 4, it is characterized in that, the general structure of the cyclic carbonate are as follows:Wherein, R1And R2It independently is the alkyl that H, C atomicity are 1~10, the alcohol that C atomicity is 1~10
Any one in the esters that the acids or C atomicity that class, C atomicity are 1~10 are 1~10；
Preferably, the reaction product is epoxide, general structure are as follows:Wherein R1And R2It is independent
Ground be H, C atomicity be 1~10 alkyl, C atomicity be 1~10 alcohols, C atomicity be 1~10 acids or C atomicity
For any one in 1~10 esters.
6. method according to claim 4 or 5, which is characterized in that the raw material further includes solvent and catalyst；
Preferably, the solvent includes any one in alkane, alkane derivatives, benzene, benzene derivative or ionic liquid or at least
Two kinds of combination；
Preferably, the catalyst includes alkaline earth oxide and/or transition metal oxide；
Preferably, the carrier of the catalyst includes any one in silica, aluminium oxide or molecular sieve or at least two
Combination；
Preferably, it is 5~100wt%, preferably 20~90wt% that the cyclic carbonate, which accounts for the mass fraction of raw material,；
Preferably, it is 0~95wt%, preferably 20~60wt% that the solvent, which accounts for the mass fraction of raw material,；
Preferably, it is 0~50wt%, preferably 0~10wt% that the catalyst, which accounts for the mass fraction of raw material,.
7. according to the described in any item methods of claim 4-6, which is characterized in that the temperature of the pyrolysis be 50~
350 DEG C, preferably 100~250 DEG C；
Preferably, the pyrolysis carries out in Reaction Separation unit.
8. according to the described in any item methods of claim 4-7, which is characterized in that absolute pressure after the vacuum control unit is adjusted
Power is 1~105Pa, preferably 200~105Pa。
9. according to the described in any item methods of claim 4-8, which is characterized in that the reaction product is collected to collection of products list
In member；
Preferably, the unreacting material includes solvent, catalyst and unreacted cyclic carbonate；
Preferably, the unreacting material enters recovery unit.
10. according to the described in any item methods of claim 4-9, which is characterized in that the described method includes: by cyclic carbonate,
Solvent and catalyst are heated to 50~350 DEG C after Reaction Separation unit is added, by vacuum control unit adjust pressure to 1~
105Pa is collected after reaction product vaporization into collection of products unit, and solvent, catalyst and unreacted cyclic carbonate enter
Recovery unit.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2019103196350 | 2019-04-19 | ||
| CN201910319635 | 2019-04-19 |
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| CN110156724A true CN110156724A (en) | 2019-08-23 |
| CN110156724B CN110156724B (en) | 2021-03-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113058382A (en) * | 2021-02-23 | 2021-07-02 | 中国科学院过程工程研究所 | Recovery device system and recovery method for effective components in tail gas |
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| CN106588863A (en) * | 2016-12-05 | 2017-04-26 | 东营市海科新源化工有限责任公司 | System and process for preparing cyclic carbonate by using composite ionic liquid catalyst |
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| CN85108659A (en) * | 1984-10-25 | 1986-07-16 | 哈尔康·斯迪集团公司 | Produce the method for alkylene oxide by alkylene carbonate |
| CN101519390A (en) * | 2008-02-28 | 2009-09-02 | 中国科学院大连化学物理研究所 | Method for preparing propylene oxide |
| CN106588863A (en) * | 2016-12-05 | 2017-04-26 | 东营市海科新源化工有限责任公司 | System and process for preparing cyclic carbonate by using composite ionic liquid catalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113058382A (en) * | 2021-02-23 | 2021-07-02 | 中国科学院过程工程研究所 | Recovery device system and recovery method for effective components in tail gas |
| CN113058382B (en) * | 2021-02-23 | 2022-06-21 | 中国科学院过程工程研究所 | Recovery device system and recovery method for effective components in tail gas |
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