CN207987065U - Low temperature Total continuity reaction system - Google Patents
Low temperature Total continuity reaction system Download PDFInfo
- Publication number
- CN207987065U CN207987065U CN201820047935.9U CN201820047935U CN207987065U CN 207987065 U CN207987065 U CN 207987065U CN 201820047935 U CN201820047935 U CN 201820047935U CN 207987065 U CN207987065 U CN 207987065U
- Authority
- CN
- China
- Prior art keywords
- quenched
- product
- import
- reaction
- low temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a kind of low temperature Total continuity reaction system.The low temperature Total continuity reaction system includes：Low temperature successive reaction unit has the outlet of crude product system；Unit continuously is quenched, there is the import of crude product system and product exit is quenched, the outlet of crude product system is connected with crude product system import；Continuous liquid separation unit, has and product inlet and product outlet is quenched, product exit is quenched and is connected with product inlet is quenched；And continuous film upgrading unit, there is crude product import and product exit, product outlet to be connected with crude product import.Low-temp reaction is realized using low temperature successive reaction unit so that reaction temperature is more mild, preferably controls the generation of by-product and impurity, improves the purity and yield of product；Substance after low-temp reaction is continuously post-processed by unit, continuous liquid separation unit and continuous film upgrading unit continuously is quenched so that target product can be detached in time, improve the yield of separative efficiency and target product.
Description
Technical field
The utility model is related to technical field of organic synthesis, in particular to a kind of low temperature Total continuity reaction system.
Background technology
For relatively traditional chemical plant installations, the continuous chemistry that flows is a revolutionary technology for overturning traditional chemical industry, it
Brand-new high-efficiency precision is opened for medication chemistry industry and refines the epoch, is the transition and upgrade of pharmaceuticals industry, is promoted innovation ability, reality
Existing " zero-emission, green, sustainable development " provides effective technological means.
Continuous flow reactor provides an efficient tool for this target.The more traditional autoclave of continuous flow reactor
For reactor, have large specific surface area, delivery rate are high, time of contact is short, by-product is few, conversion ratio higher, good operability,
Each condition of safe, quick the advantages that directly amplifying, continuous flow reaction are (reactant, product, by-product, catalyst, molten
Agent, medium) milligram ammonia, the reaction conditions such as temperature, pressure can carry out more accuracy controlling, (intermittently anti-compared to traditional batch reaction
Answer), during reaction amplification and optimization, there is higher reaction efficiency, higher reproducibility and stability.And continuous flow is reacted
Utensil have low heat buffer requirement amount, output increased, reagent reduce, the degree of automation is high and greatlys save human resources
Advantage.
In field of medicaments, traditional batch processes still reaction technology is substituted using continuous flow reaction technology, is being obtained
To each pharmaceuticals great attention and rapidly developing.And in medical synthesis field, post-processing technology is but still kept
Its initial state, is a kind of intermittent batch processes, that is, needs to use traditional reaction kettle, to the mixing after reaction
Object such as is extracted, is washed, being concentrated, being dried, being crystallized at the post-processing operations.This traditional, inefficient intermittent aftertreatment technology,
Bottleneck is formed to efficient continuous reaction technology, urgent need will be improved.
Utility model content
The main purpose of the utility model is to provide a kind of low temperature Total continuity reaction systems, to solve in the prior art
The low problem of low-temp reaction efficiency of post treatment.
To achieve the goals above, one side according to the present utility model provides a kind of low temperature Total continuityization reaction
System, including：Low temperature successive reaction unit has the outlet of crude product system；Unit continuously is quenched, there is crude product system import
Be quenched product exit, the outlet of crude product system is connected with crude product system import；Continuous liquid separation unit, have be quenched product into
Mouth and product outlet, are quenched product exit and are connected with product inlet is quenched；And continuous film upgrading unit, there is crude product
Import and product exit, product outlet are connected with crude product import.
Further, above-mentioned continuous unit is quenched to include：Reaction unit is quenched in level-one, with the first quencher entrance, just
Product exit and crude product system import is quenched；Reaction unit is quenched in two level, have the second quencher entrance, be just quenched product into
Mouthful and product exit is quenched, product exit is just quenched and product inlet is quenched is connected with first；First quencher feeding mechanism, with first
Quencher entrance is pumped by third automatic feed to be connected；Second quencher feeding mechanism passes through the 4th with the second quencher entrance
Automatic feed pump is connected.
Further, it is the second coil reactor that reaction unit, which is quenched, in above-mentioned level-one, and preferably the second coil reactor has
Second temperature controller；It is preferred that it is successive reaction kettle that reaction unit, which is quenched, in two level, further preferred successive reaction kettle is provided with the
Three temperature controllers.
Further, above-mentioned continuous liquid separation unit includes：There is continuous liquid separation column the first organic phase outlet, water phase to export
With product inlet is quenched, be quenched product exit be quenched product inlet by the 5th automatic feed pump be connected；Continuous extraction detaches
There is column extractant import, water phase import and Second Organic Phase outlet, water phase outlet to pass through the 6th automatic feed with water phase import
Pump is connected；Organic phase caches storage tank, has the first organic phase import and a product outlet, the first organic phase outlet, second organic
Mutually outlet is connected with the first organic phase import, and extractant feeding mechanism is connected with extractant import；It is preferred that continuous liquid separation column has
4th temperature controller, preferably continuous extraction splitter have the 5th temperature controller.
Further, above-mentioned continuous film upgrading unit includes：Continuous drying column has drier import, third organic
Mutually outlet and crude product import, product outlet are connected with crude product import by the 7th automatic feed pump；Continuous film evaporates
Device has Second Organic Phase import and product exit, third organic phase outlet automatic by the 8th with Second Organic Phase import
Feed pump is connected.
Further, above-mentioned continuous film upgrading unit further includes drier device without interruption, and drier is without interruption
Device is connected with drier import.
Further, above-mentioned drier device without interruption is screw feeder；It is preferred that continuous drying column has the 6th temperature
Spend controller.
Further, above-mentioned continuous film vaporising device includes：First continuous film evaporator, have Second Organic Phase into
Mouth and the 4th organic phase outlet；There is second continuous film evaporator the import of third organic phase, azeotropic solvent import and product to go out
Mouthful, the 4th organic phase outlet is connected with the import of third organic phase by the 9th automatic feed pump；Azeotropic solvent feeding mechanism, together
It boils solvent inlet and is pumped by the tenth automatic feed and is connected.
Further, above-mentioned first continuous film evaporator has the 7th temperature controller, the second continuous film evaporator
With the 8th temperature controller.
Further, above-mentioned low temperature successive reaction unit includes：First feedstock supply unit；Quick property metal reagent supply dress
It sets；Low temperature continuous reaction apparatus has the first material inlet, quick property metal reagent import and the outlet of crude product system, and first is former
Material feeding mechanism is connected with the first material inlet by the first automatic feed pump, quick property metal reagent feeding mechanism and quick property metal
Reagent entry port is pumped by the second automatic feed to be connected；It is preferred that low temperature continuous reaction apparatus is the first coil reactor, it is further excellent
Select the first coil reactor that there is the first temperature controller.
Using the technical solution of the utility model, which includes low temperature successive reaction unit,
I.e. utilize successive reaction technology realize low-temp reaction, effectively increase the thermal energy of low-temp reaction with further such that reaction temperature more
To be mild, the generation of by-product and impurity is preferably controlled, the purity and yield of product are improved；Substance warp after low-temp reaction
It crosses and unit, continuous liquid separation unit and continuous film upgrading unit is continuously quenched continuously is post-processed so that low-temp reaction
The target product obtained afterwards can be detached in time, avoid increasing for by-product caused by product accumulation, and then improve
The yield of separative efficiency and target product, and since by-product and impurity are reduced, the energy of purification of products consumption and examination
The cost for energy consumption, waste discharge and the processing that agent also reduces, reduces purification of products.Meanwhile low temperature Total continuity reaction system
The application of system so that equipment operation is easy, the safety is improved, and the working strength of operator reduces, cost of labor also reduces.
Description of the drawings
The accompanying drawings which form a part of this application are used to provide a further understanding of the present invention, this practicality
Novel illustrative embodiments and their description are not constituted improper limits to the present invention for explaining the utility model.
In the accompanying drawings：
Fig. 1 shows that the structure for the low temperature Total continuity reaction system that a kind of embodiment according to the present utility model provides is shown
It is intended to；And
Fig. 2 shows the structures for the low temperature Total continuity reaction system that another embodiment according to the present utility model provides
Schematic diagram.
Wherein, above-mentioned attached drawing includes the following drawings label：
10, low temperature successive reaction unit；11, the first feedstock supply unit；12, quick property metal reagent feeding mechanism；13, low
Warm continuous reaction apparatus；14, the first automatic feed pumps；15, the second automatic feed pumps；
20, unit is continuously quenched；21, reaction unit is quenched in level-one；22, reaction unit is quenched in two level；23, the first quencher
Feeding mechanism；24, the second quencher feeding mechanism；25, third automatic feed pumps；26, the 4th automatic feed pump；
30, continuous liquid separation unit；31, continuous liquid separation column；32, continuous extraction splitter；33, organic phase caches storage tank；34、
Extractant feeding mechanism；35, the 5th automatic feed pumps；36, the 6th automatic feed pumps；
40, continuous film upgrading unit；41, continuous drying column；42, continuous film vaporising device；43, drier continuously supplies
Answer device；421, the first continuous film evaporator；422, the second continuous film evaporator；423, azeotropic solvent feeding mechanism；44、
7th automatic feed pumps；45, the 8th automatic feed pumps；46, the 9th automatic feed pumps；47, the tenth automatic feed pumps.
Specific implementation mode
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The utility model will be described in detail below with reference to the accompanying drawings and embodiments.
As the application background technology is analyzed, the post-processing of the medical synthetic technology of the prior art uses interval batch work
Skill leads to the problem that efficiency of post treatment is relatively low, in order to solve this problem, this application provides low temperature Total continuity reaction system and
Using.
In a kind of typical embodiment of the application, a kind of low temperature Total continuity reaction system is provided, such as Fig. 1 institutes
Show, which includes low temperature successive reaction unit 10, unit 20, continuous liquid separation unit 30 continuously is quenched
And continuous film upgrading unit 40, low temperature successive reaction unit 10 are exported with crude product system；It is continuous that the tool of unit 20 is quenched
There is the import of crude product system and product exit is quenched, the outlet of crude product system is connected with crude product system import；Continuous liquid separation list
Member 30, which has, is quenched product inlet and product outlet, and product exit is quenched and is connected with product inlet is quenched；Continuous film concentrates
There is unit 40 crude product import and product exit, product outlet to be connected with crude product import.
The low temperature Total continuity reaction system of the application includes low temperature successive reaction unit 10, that is, utilizes successive reaction technology
It realizes low-temp reaction, effectively increases the thermal energy of low-temp reaction further such that reaction temperature is more mild, preferably to control
The generation of by-product and impurity improves the purity and yield of product；Substance after low-temp reaction by be continuously quenched unit 20,
Continuous liquid separation unit 30 and continuous film upgrading unit 40 are continuously post-processed so that the target obtained after low-temp reaction
Product can be detached in time, avoid increasing for by-product caused by product accumulation, and then improve separative efficiency and mesh
The yield of product is marked, and since by-product and impurity are reduced, the energy and reagent of purification of products consumption are also reduced, dropped
The low energy consumption of purification of products, waste discharge and the cost of processing.Meanwhile the application of low temperature Total continuity reaction system to set
For easy to operate, the safety is improved, the working strength of operator reduces, cost of labor also reduces.
Preferably, as shown in Fig. 2, above-mentioned continuous be quenched that reaction unit 21 is quenched including level-one in unit 20, two level is quenched instead
Answer device 22, the first quencher feeding mechanism 23 and the second quencher feeding mechanism 24, reaction unit 21, which is quenched, in level-one has the
Product exit and crude product system import is just quenched in one quencher entrance；Reaction unit 22, which is quenched, in two level has the second quencher
Entrance is just quenched product inlet and product exit is quenched, and product exit is just quenched and just product inlet is quenched is connected；First is quenched
Agent feeding mechanism 23 is connected with the first quencher entrance by third automatic feed pump 25；Second quencher feeding mechanism 24 and
Two quencher entrances are connected by the 4th automatic feed pump 26.First quencher entrance therein and the import of crude product system can be with
For the same mouth.
Realization being steadily quenched step by step to low-temp reaction is quenched by the way that two-stage is arranged, wherein utilize third automatic feed
Pump 25 is quenched reaction unit 21 to level-one and carries out Automatic-feeding, and reaction unit 22 is quenched to two level using the 4th automatic feed pump 26
Automatic-feeding is carried out, realizes the accurate feeding of quencher, is conducive to that speed is quenched according to real reaction adjustment.
Above-mentioned level-one is quenched reaction unit 21 and two level be quenched reaction unit 22 may be used it is common using the prior art
Continuous reacting device, in a kind of embodiment of the application, it is the second coil reactor that reaction unit 21, which is quenched, in above-mentioned level-one, excellent
Select the second coil reactor that there is second temperature controller；Reaction unit 21 is quenched as level-one using the second coil reactor,
Using the characteristics of coil reactor quencher and the complete material of unreacted are more fully contacted, realization is quickly quenched
Reaction, and second temperature controller is provided in the second coil reactor, it is further increased and is quenched by implementation adjustment temperature
Efficiency.Furthermore it is preferred that it is successive reaction kettle that reaction unit 22, which is quenched, in two level, further preferred successive reaction kettle is provided with third temperature
Spend controller.Have been completed that the major part to low temperature successive reaction is quenched since reaction is quenched in level-one, using continuous anti-
It answers kettle that reaction unit 22 is quenched as two level and being continuously quenched for low cost can be realized；It is further advanced by third temperature controller
The temperature of successive reaction kettle is controlled, realization is accurately controlled to extent of reaction is quenched, and reaction efficiency is quenched in raising, and it is unnecessary to reduce
Quencher waste.
Above-mentioned continuous liquid separation unit 30 can adjust its specific structure composition according to specific reaction, preferably such as Fig. 2
Shown, above-mentioned continuous liquid separation unit 30 includes continuous liquid separation column 31, continuous extraction splitter 32, organic phase caching storage tank 33 and extraction
It takes agent feeding mechanism 34, continuous liquid separation column 31 that there is the first organic phase outlet, water phase outlet and product inlet is quenched, product is quenched
It exports and product inlet is quenched 35 is connected by the 5th automatic feed pump；Continuous extraction splitter 32 has extractant import, water
Phase import and Second Organic Phase outlet, water phase outlet are connected with water phase import by the 6th automatic feed pump 36；Organic phase caches
Storage tank 33 has the first organic phase import and product outlet, the first organic phase outlet, Second Organic Phase outlet and first organic
Phase import is connected, and extractant feeding mechanism 34 is connected with extractant import.Divided product is quenched using continuous liquid separation column 31
Liquid, to realize the initial gross separation of organic phase and water phase in the case where any reagent need not be added；Then continuous extraction is utilized
It takes splitter 32 to carry out extraction and separation organic phase therein to water phase, realizes the further recycling to target product.In order to improve
There is the 4th temperature controller, preferably continuous extraction splitter 32 to have the 5th temperature for separative efficiency, preferably continuous liquid separation column 31
Controller.
Above-mentioned continuous film upgrading unit 40 is used for the organic phase isolated to continuous liquid separation unit 30 into traveling one
Separating-purifying processing is walked, preferably as shown in Fig. 2, above-mentioned continuous film upgrading unit 40 includes continuous drying column 41 and continuous film
Vaporising device 42, continuous drying column 41 have drier import, third organic phase outlet and crude product import, product outlet with
Crude product import is connected by the 7th automatic feed pump 44；Continuous film vaporising device 42 has Second Organic Phase import and product
Outlet, third organic phase outlet are connected with Second Organic Phase import by the 8th automatic feed pump 45.Using above-mentioned continuous drying
Column 41 carries out absorption processing to the remaining water phase in organic phase, to improve the purity of organic phase；Then continuous film is utilized
Vaporising device 42 carries out continuous evaporation process to the organic phase after purification, by efficient, high-purity separation characteristic of thin film evaporation,
Realization efficiently separates product.
For the ease of adjusting the usage amount of drier according to the aqueous-phase concentration in organic phase, preferably above-mentioned continuous film concentration
Unit 40 further includes drier device 43 without interruption, and drier device 43 without interruption is connected with drier import.Using dry
Drying prescription device 43 without interruption continuously supplies drier, and realizes drier dosage by adjusting the supply rate of drier
Adjustment, to improve the utilization ratio of drier.
It is preferred that above-mentioned drier device 43 without interruption supplies drier, drier preferably wherein is solid drier,
And then preferably above-mentioned drier device 43 without interruption is screw feeder.Further, in order to improve drier to organic phase
The adsorption effect of middle water phase, preferably continuous drying column 41 have the 6th temperature controller, to adjust adsorption temp, improve drier
Adsorption effect.
In the application another kind embodiment, as shown in Fig. 2, above-mentioned continuous film vaporising device 42 includes first continuous thin
Film evaporator 421, the second continuous film evaporator 422 and azeotropic solvent feeding mechanism 423, the first continuous film evaporator 421
With Second Organic Phase import and the 4th organic phase outlet；Second continuous film evaporator 422 has the import of third organic phase, is total to
Solvent inlet and product exit are boiled, the 4th organic phase outlet is connected with the import of third organic phase by the 9th automatic feed pump 46；
Azeotropic solvent feeding mechanism 423 is connected with azeotropic solvent import by the tenth automatic feed pump 47.It is continuous thin by setting first
Film evaporator 421 is evaporated processing to the organic phase after drying, to carry out purification processes to target product, then again by setting
The second continuous film evaporator 422 is set, further evaporation process is carried out to organic phase in the case of being participated in using entrainer, it is real
Now to the purification of target product.Above-mentioned entrainer is implemented to provide by entrainer feeding mechanism, and then ensure that second is continuous thin
The stabilization of film evaporator 422 is carried out continuously.Above-mentioned entrainer import and the import of third organic phase can be same import.
Preferably, above-mentioned first continuous film evaporator 421 has the 7th temperature controller, the second continuous film evaporator
422 have the 8th temperature controller.To control the temperature of thin film evaporation, the purification efficiency of target product is improved.
The low temperature Total continuity reaction system of the application is applied to a variety of low-temp reactions, is particularly suitable for quick property metal reagent
The low-temp reaction of participation, preferably as shown in Fig. 2, above-mentioned low temperature successive reaction unit 10 includes the first feedstock supply unit 11, quick
Property metal reagent feeding mechanism 12 and low temperature continuous reaction apparatus 13, low temperature continuous reaction apparatus 13 have the first material inlet,
Quick property metal reagent import and the outlet of crude product system, the first feedstock supply unit 11 and the first material inlet are automatic by first
Feed pump 14 is connected, and quick property metal reagent feeding mechanism 12 pumps 15 phases with quick property metal reagent import by the second automatic feed
Even.The charging rate of the reactant of reaction is participated in using above-mentioned first automatic feed pump 14 and 15 control of the second automatic feed pump,
And then the retention time of low temperature reaction is adjusted with this, while according to above-mentioned first automatic feed pump 14 and the second automatic feed
The speed of the follow-up each automatic feed pump of charging rate adjustment of pump 15 is adapted with it.
Furthermore it is preferred that low temperature continuous reaction apparatus 13 is the first coil reactor, further preferred first coil reactor
With the first temperature controller.Certainly, above-mentioned low temperature continuous reaction apparatus 13 or successive reaction kettle, using the first coil pipe
The advantage of reactor is that the contact of material is more preferable, reaction efficiency higher.
In order to make those skilled in the art more easily use above system, in another typical embodiment of the application
In, provide a kind of application of any of the above-described kind of low temperature Total continuity reaction system in the reaction of low temperature Total continuityization.
When the low temperature Total continuity reaction system of the application is applied in the reaction of low temperature Total continuityization, successive reaction is utilized
Technology realizes low-temp reaction, effectively increases the thermal energy of low-temp reaction with further such that reaction temperature is more mild, preferably
The generation for controlling by-product and impurity, improves the purity and yield of product；Substance after low-temp reaction is by being continuously quenched list
Member 20, continuous liquid separation unit 30 and continuous film upgrading unit 40 are continuously post-processed so that are obtained after low-temp reaction
Target product can be detached in time, avoid increasing for by-product caused by product accumulation, so improve separation effect
The yield of rate and target product, and since by-product and impurity are reduced, the energy and reagent of purification of products consumption also subtract
Less, energy consumption, waste discharge and the cost of processing of purification of products are reduced.Meanwhile low temperature Total continuity reaction system is answered
With so that equipment operation is easy, the safety is improved, the working strength of operator reduces, cost of labor also reduces.
Preferably, above application include diisobutyl aluminium hydride reduction trifluoroacetic acid ethyl ester prepare the reaction of trifluoropropanol with
And last handling process, wherein diisobutyl aluminium hydride is quick property metal reagent.Due to using low temperature Total continuity reaction system into
The above-mentioned reaction of row, therefore the utilization ratio of heat can be improved, preferably diisobutyl aluminium hydride restores going back for trifluoroacetic acid ethyl ester
Former temperature is -30~0 DEG C.
The workflow of above-mentioned low temperature Total continuity reaction system is illustrated below with reference to Fig. 2, first first is former
Expect the material solution in feeding mechanism 11 and quick property metal reagent in quick property metal reagent feeding mechanism 12 simultaneously by first from
14 and second automatic feed of dynamic feed pump pump 15 is pumped into low temperature continuous reaction apparatus 13 (the i.e. first continuous coil reactor) respectively
In, low temperature continuous reaction apparatus 13 controls the temperature of low temperature continuous reaction apparatus 13 by the first temperature controller, to ensure to reach
To the temperature of technological requirement.Mixture from low temperature continuous reaction apparatus 13 out enters level-one and reaction unit 21 is quenched, together
When enter also have the first quencher, be quenched for excessive quick property metal reagent to be carried out level-one.Reaction unit is quenched in level-one
21 ensure reaction in Process temperature ranges by its second temperature controller.Out mixed is quenched in reaction unit 21 from level-one
Conjunction object enters two level and reaction unit 22 is quenched, while what is entered also has the second quencher, and the first quencher and the second quencher can
With identical, for further quick property metal reagent to be thoroughly quenched, while by the inorganic matter in system from reaction organic phase
In wash in water phase, reaction temperature can be controlled by third temperature controller.It is logical that the system in reaction unit 22 is quenched in two level
The 5th automatic feed pump 35 to be crossed to be transferred in continuous liquid separation column 31 and carry out continuous liquid separation, lower water mutually continuously enters water phase storage tank,
Upper organic phase continuously enters organic phase caching storage tank 33.Continuous liquid separation column 31 passes through the 4th temperature controller temperature control.Water phase is stored up
Water phase in tank is continuously transferred in continuous extraction splitter 32 by the 6th automatic feed pump 36, while being pumped by continuously pumping
Extractant.The temperature of continuous extraction splitter 32 carries out temperature control by substrate temperature controller, in continuous extraction splitter 32
In, it after water phase is further extracted, flows continually out into wastewater storage tank, the organic phase after extraction then continuously enters organic phase caching
Storage tank 33.Organic phase in organic phase caching storage tank 33 is continuously transferred to continuous drying column 41 by the 7th automatic feed pump 44
In, meanwhile, solid drier is continuously added to do organic phase in continuous drying column 41 by drier device 43 without interruption
Dry, 41 temperature of continuous drying column is controlled by the 6th temperature controller.In continuous drying column 41 water is formed after dry water suction
Phase is continuously discharged from dry column bottom liquid outlet, and organic phase is continuously discharged into drying by 41 upper layer liquid outlet of continuous drying column
Organic phase storage tank afterwards.Organic phase in organic phase storage tank is pumped into the first continuous film evaporator 421 by the 8th automatic feed pump 45,
Its thickening temperature is controlled by the 7th temperature controller.Organic phase enters storage tank after the concentration of the first continuous film evaporator 421,
In organic phase continuously enter the second continuous film evaporator 422 through the 9th automatic feed pump 46, while what is entered also has azeotropic
Solvent supply unit 423 is pumped into the entrainer of the second continuous film evaporator 422 by the tenth automatic feed pump 47.Second is continuous
The effect of thin film evaporator 422 is that product is further dried to qualification by entrainer azeotropic dehydration, and the second continuous film steams
The thickening temperature of hair device 422 is controlled by the 8th temperature controller.Liquid in second continuous film evaporator 422 out is most
Qualified product eventually, is received by receiving tank.
The advantageous effect of the application is further illustrated below with reference to embodiment and comparative example.
Trifluoropropanol is prepared with diisobutyl aluminium hydride reduction trifluoroacetic acid ethyl ester, reaction route is as follows：
Embodiment 1
Above-mentioned reaction is carried out using continuous production processes, continuous production processes are implemented using system shown in Fig. 2, wherein
The molar ratio of diisobutyl aluminium hydride and trifluoroacetic acid ethyl ester is 1.25, and the quencher being quenched for the first time is ethyl alcohol, quencher
Dosage is 5.0 equivalents, and it is 20 DEG C that temperature, which is quenched,；The quencher being quenched for the second time is 10% aqueous sulfuric acid, the dosage of quencher
For 2.5 equivalents, it is 20 DEG C that temperature, which is quenched,；The temperature of first time liquid separation is 20 DEG C；The temperature for extracting liquid separation is 20 DEG C, and extractant is
2- methyltetrahydrofurans, Solvent quantity are 5~10mL/g relative to trifluoroacetic acid ethyl ester；The temperature of dry liquid separation is 20 DEG C,
Drier is anhydrous magnesium sulfate, and drier dosage is 1.0g/g relative to trifluoroacetic acid ethyl ester；First time film thickening temperature is
25 DEG C, concentration vacuum degree is -0.09MPa；Second of film thickening temperature is 20 DEG C, and concentration vacuum degree is -0.09, and entrainer is
Ethyl alcohol, it is 3g/L that the dosage of entrainer, which is relative to trifluoroacetic acid ethyl ester,.
Embodiment 2
Above-mentioned reaction is carried out using continuous production processes, continuous production processes are implemented using system shown in Fig. 2, wherein
The molar ratio of diisobutyl aluminium hydride and trifluoroacetic acid ethyl ester is 1.05, and the quencher being quenched for the first time is ethyl alcohol, quencher
Dosage is 6.0 equivalents, and it is 0 DEG C that temperature, which is quenched,；The quencher being quenched for the second time is 10% aqueous sulfuric acid, and the dosage of quencher is
1.5 equivalents, it is 30 DEG C that temperature, which is quenched,；The temperature of first time liquid separation is 30 DEG C；The temperature for extracting liquid separation is 30 DEG C, extractant 2-
Methyltetrahydrofuran, Solvent quantity are 5mL/g relative to trifluoroacetic acid ethyl ester；The temperature of dry liquid separation is 10 DEG C, drier
For no anhydrous sodium sulfate, drier dosage is 1.5g/g relative to trifluoroacetic acid ethyl ester；First time film thickening temperature is 30 DEG C,
Concentration vacuum degree is -0.08MPa；Second of film thickening temperature is 30 DEG C, and concentration vacuum degree is -0.08MPa, and entrainer is second
Alcohol, it is 1g/L that the dosage of entrainer, which is relative to trifluoroacetic acid ethyl ester,.
Embodiment 3
Above-mentioned reaction is carried out using continuous production processes, continuous production processes are implemented using system shown in Fig. 2, wherein
The molar ratio of diisobutyl aluminium hydride and trifluoroacetic acid ethyl ester is 1.50, and the quencher being quenched for the first time is ethyl alcohol, quencher
Dosage is 3.0 equivalents, and it is 30 DEG C that temperature, which is quenched,；The quencher being quenched for the second time is 10% aqueous sulfuric acid, the dosage of quencher
For 3.0 equivalents, it is 0 DEG C that temperature, which is quenched,；The temperature of first time liquid separation is 10 DEG C；The temperature for extracting liquid separation is 10 DEG C, and extractant is
2- methyltetrahydrofurans, Solvent quantity are 10mL/g relative to trifluoroacetic acid ethyl ester；The temperature of dry liquid separation is 30 DEG C, dry
Agent is Anhydrous potassium carbonate, and drier dosage is 0.5g/g relative to trifluoroacetic acid ethyl ester；First time film thickening temperature is 15 DEG C,
Concentration vacuum degree is -0.1MPa；Second of film thickening temperature is 15 DEG C, and concentration vacuum degree is -0.1MPa, and entrainer is second
The dosage of alcohol, entrainer is relative to trifluoroacetic acid ethyl ester 4g/L.
Comparative example 1
Implemented with 1 identical process of embodiment using batch production technology, wherein other than reaction temperature is different, it is other each
Parameter is same as Example 1.
The reaction time of two kinds of technique and temperature are as shown in the table：
Can be seen that according to above-mentioned comparison can improve product using the low temperature Total continuity reaction system of the application receives
Rate, and shorten the reaction time, i.e., the efficiency of post-processing is improved relative to batch reaction.
It can be seen from the above description that the above embodiments of the present invention achieve the following technical effects：
The low temperature Total continuity reaction system of the application includes low temperature successive reaction unit, that is, utilizes successive reaction technology real
Existing low-temp reaction effectively increases the thermal energy of low-temp reaction so that further such that reaction temperature is more mild, preferably control is secondary
The generation of product and impurity improves the purity and yield of product；Substance after low-temp reaction is by being continuously quenched unit, continuous
Liquid separation unit and continuous film upgrading unit are continuously post-processed so that the target product obtained after low-temp reaction can
It is detached in time, avoids increasing for by-product caused by product accumulation, and then improve separative efficiency and target product
Yield, and since by-product and impurity are reduced, the energy and reagent of purification of products consumption also reduce, reduce product
Energy consumption, waste discharge and the cost of processing of purification.Meanwhile the application of low temperature Total continuity reaction system so that equipment operation is simple
Just, the safety is improved, and the working strength of operator reduces, cost of labor also reduces.
The above descriptions are merely preferred embodiments of the present invention, is not intended to limit the utility model, for this
For the technical staff in field, various modifications and changes may be made to the present invention.It is all in the spirit and principles of the utility model
Within, any modification, equivalent replacement, improvement and so on should be included within the scope of protection of this utility model.
Claims (11)
1. a kind of low temperature Total continuity reaction system, which is characterized in that including：
Low temperature successive reaction unit (10) has the outlet of crude product system；
Unit (20) continuously is quenched, there is the import of crude product system and product exit is quenched, the crude product system outlet and institute
Crude product system import is stated to be connected；
Continuous liquid separation unit (30), has and product inlet and product outlet is quenched, the product exit that is quenched is quenched with described
Product inlet is connected；And
Continuous film upgrading unit (40) has crude product import and product exit, the product outlet and the crude product
Import is connected.
2. low temperature Total continuity reaction system according to claim 1, which is characterized in that described that unit (20) continuously is quenched
Including：
Reaction unit (21) is quenched in level-one, have the first quencher entrance, be just quenched product exit and the crude product system into
Mouthful；
Reaction unit (22) is quenched in two level, have the second quencher entrance, be just quenched product inlet and it is described product exit is quenched,
It is described be just quenched product exit with it is described at the beginning of product inlet be quenched be connected；
First quencher feeding mechanism (23) is connected with the first quencher entrance by third automatic feed pump (25)；
Second quencher feeding mechanism (24) is connected with the second quencher entrance by the 4th automatic feed pump (26).
3. low temperature Total continuity reaction system according to claim 2, which is characterized in that
It is the second coil reactor that reaction unit (21), which is quenched, in the level-one.
4. low temperature Total continuity reaction system according to claim 2, which is characterized in that reaction unit is quenched in the two level
(22) it is successive reaction kettle.
5. low temperature Total continuity reaction system according to claim 1, which is characterized in that the continuous liquid separation unit (30)
Including：
Continuous liquid separation column (31), have the first organic phase outlet, water phase outlet and it is described be quenched product inlet, it is described that product is quenched
Outlet with it is described product inlet is quenched (35) is pumped by the 5th automatic feed be connected；
Continuous extraction splitter (32), has extractant import, water phase import and a Second Organic Phase outlet, water phase outlet with
The water phase import pumps (36) by the 6th automatic feed and is connected；
Organic phase caches storage tank (33), has the first organic phase import and product outlet, first organic phase outlet, described
Second Organic Phase outlet is connected with the first organic phase import,
Extractant feeding mechanism (34) is connected with the extractant import.
6. low temperature Total continuity reaction system according to claim 1, which is characterized in that the continuous film upgrading unit
(40) include：
There is continuous drying column (41) drier import, third organic phase outlet and the crude product import, the crude product to go out
Mouth pumps (44) by the 7th automatic feed with the crude product import and is connected；
Continuous film vaporising device (42) has Second Organic Phase import and the product exit, the third organic phase outlet
(45) are pumped with the Second Organic Phase import by the 8th automatic feed to be connected.
7. low temperature Total continuity reaction system according to claim 6, which is characterized in that the continuous film upgrading unit
(40) further include drier device without interruption (43), the drier device without interruption (43) and the drier import phase
Even.
8. low temperature Total continuity reaction system according to claim 7, which is characterized in that the drier dress without interruption
It is screw feeder to set (43).
9. low temperature Total continuity reaction system according to claim 6, which is characterized in that the continuous film vaporising device
(42) include：
First continuous film evaporator (421) has the Second Organic Phase import and the 4th organic phase outlet；
Second continuous film evaporator (422) has the import of third organic phase, azeotropic solvent import and the product exit, institute
It states the 4th organic phase outlet (46) is pumped by the 9th automatic feed with the third organic phase import and be connected；
Azeotropic solvent feeding mechanism (423) pumps (47) by the tenth automatic feed with the azeotropic solvent import and is connected.
10. low temperature Total continuity reaction system according to claim 1, which is characterized in that the low temperature successive reaction list
First (10) include：
First feedstock supply unit (11)；
Quick property metal reagent feeding mechanism (12)；
There is low temperature continuous reaction apparatus (13) the first material inlet, quick property metal reagent import and the crude product system to go out
Mouthful, first feedstock supply unit (11) pumps (14) by the first automatic feed with first material inlet and is connected, described
Quick property metal reagent feeding mechanism (12) pumps (15) by the second automatic feed with the quick property metal reagent import and is connected.
11. low temperature Total continuity reaction system according to claim 10, which is characterized in that the low temperature successive reaction dress
It is the first coil reactor to set (13).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820047935.9U CN207987065U (en) | 2018-01-11 | 2018-01-11 | Low temperature Total continuity reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820047935.9U CN207987065U (en) | 2018-01-11 | 2018-01-11 | Low temperature Total continuity reaction system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207987065U true CN207987065U (en) | 2018-10-19 |
Family
ID=63819206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201820047935.9U Active CN207987065U (en) | 2018-01-11 | 2018-01-11 | Low temperature Total continuity reaction system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN207987065U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117801044A (en) * | 2024-02-29 | 2024-04-02 | 天津凯莱英医药科技发展有限公司 | Continuous production method and device for progesterone |
| CN117801044B (en) * | 2024-02-29 | 2024-07-09 | 天津凯莱英医药科技发展有限公司 | Continuous production method and device for progesterone |
-
2018
- 2018-01-11 CN CN201820047935.9U patent/CN207987065U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117801044A (en) * | 2024-02-29 | 2024-04-02 | 天津凯莱英医药科技发展有限公司 | Continuous production method and device for progesterone |
| CN117801044B (en) * | 2024-02-29 | 2024-07-09 | 天津凯莱英医药科技发展有限公司 | Continuous production method and device for progesterone |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108129267A (en) | Low temperature Total continuity reaction system and application | |
| CN102557932B (en) | Method for producing isobutyl acetate | |
| CN105237369A (en) | Isoborneol-dehydrogenated camphor refining method and equipment therefor | |
| CN110947348A (en) | Micro-channel continuous ozone oxidation device | |
| CN109534971B (en) | 5-chloro-indanone production device and production method thereof | |
| CN108640838B (en) | Device and method for continuously producing dibutyl phthalate | |
| CN207987065U (en) | Low temperature Total continuity reaction system | |
| CN109806816A (en) | A kind of chlorination reaction device of continuous round-robin method production | |
| CN216513614U (en) | Efficient 4-chlorine-3 ',4' -dimethoxy benzophenone apparatus for producing | |
| CN207143010U (en) | The dehydration device of esterification products under a kind of acid condition | |
| CN112409199B (en) | Continuous production process and device for amino acid methyl ester | |
| CN211800862U (en) | Continuous esterification reaction device | |
| CN216172263U (en) | Reaction device for synthesizing alpha-acetyl-gamma-butyrolactone | |
| CN106478340B (en) | It is a kind of based on rectifying tower with bulkhead Separation of Benzene-olefinic system system | |
| CN212246660U (en) | Device for extracting high-purity sodium acrylate or sodium methacrylate from UV monomer production wastewater | |
| CN209791506U (en) | chlorination reaction device for continuous circulation production | |
| CN208182893U (en) | A kind of system for continuous esterification production ethyl cyanoacetate | |
| CN113274751A (en) | Preparation system of potassium persulfate | |
| CN102964237A (en) | Method and equipment for preparing copper acetate by using nitric acid catalytic oxidation method | |
| CN202766441U (en) | Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein | |
| CN207775122U (en) | A kind of device for realizing that formic acid glycol ester is applied mechanically in metronidazole production | |
| CN205420234U (en) | Synthetic and result separator of nitromethane | |
| CN202072483U (en) | Preparation device of ammonium nitrate concentrated solution | |
| CN217450115U (en) | Production system of 8-chloro-6-oxo-ethyl octanoate | |
| CN203155228U (en) | Nitrating pot with automatic overflow function |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |