CN110256223A - A method of 1- (1- chlorine cyclopropyl) ethyl ketone is prepared using micro passage reaction - Google Patents
A method of 1- (1- chlorine cyclopropyl) ethyl ketone is prepared using micro passage reaction Download PDFInfo
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Abstract
The present invention provides a kind of method for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction, preheating, 3 after the mixing and mixing of raw material a and catalyst, the preheating of chloro- 2 pentanone of 5- bis- pump, raw material a and 3, the cyclization of chloro- 2 pentanone of 5- bis- pump, the cooling procedure of product carry out in micro passage reaction, this method is easy to operate, the high income of feed stock conversion and product, reaction time greatly shortens, by-product is reduced, temperature in reaction process can be precisely controlled, reacts serialization.
Description
Technical field
The present invention relates to 1- (1- chlorine cyclopropyl) ethyl ketone preparation technical fields, and in particular to a kind of to utilize micro passage reaction
The method for preparing 1- (1- chlorine cyclopropyl) ethyl ketone.
Background technique
Prothioconazoles are a kind of New-type wide-spectrum triazole thioketone fungicide that Beyer Co., Ltd develops, and are mainly used for preventing and treating paddy
Numerous diseases such as class, wheat legume crop, prothioconazoles toxicity is low, no teratogenesis, mutagenesis type, to embryo's nontoxicity, to people and
Environmental security.
The molecular formula of 1- (1- chlorine cyclopropyl) ethyl ketone is C5H7ClO, molecular weight are 118.562, and structural formula is as follows, are rosickyite
The important intermediate of bacterium azoles.
1- (1- chlorine cyclopropyl) ethyl ketone is quick by chloro- 2 pentanone of 3,5- bis- mainly with chloro- 2 pentanone of 3,5- bis- for raw material at present
The reaction kettle for getting liquid alkaline ready is instilled, cyclization synthesis is carried out and is made.
Currently used is the batch production in batch reactor, and batch reactor need to have the auxiliary such as charging and discharging behaviour
Make, product quality is also not easy to stablize, and existing cannot achieve that continuous production, yield are low, side reaction is more, generation waste water is more, there have to be bright
The disadvantages of aobvious enlarge-effect.In addition, it is longer the time required to synthesis in a kettle, it will cause 1- (the 1- chlorine ring that synthesis obtains
Propyl) ethyl ketone residence time under alkaline environment is too long, and by-product is generated, cause coking extent serious.
Further, since cyclization is complicated, influence factor is more, and under low temperature, principal product is alpha-chloro cyclopentanone, and high temperature is again
Tar generation is had, therefore reaction process must be strictly controlled temperature.
The preparation method of 1- (1- chlorine cyclopropyl) ethyl ketone is single at present, rarely has micro passage reaction being applied to 1- (1- chlorine
Cyclopropyl) ethyl ketone preparation in.
Summary of the invention
For overcome the deficiencies in the prior art, it is prepared it is an object of the present invention to provide a kind of using micro passage reaction
The method of 1- (1- chlorine cyclopropyl) ethyl ketone, the micro-structure inside micro passage reaction make microreactor equipment have greatly ratio
Surface area makes it have fabulous heat transfer and mass transfer ability up to even thousands of times of hundred times of stirred tank specific surface area, can be with
Realize that the moment of material uniformly mixes and efficient heat transfer, the present invention connect and are formed in parallel using multiple micro passage reactions,
Greatly improve mixed effect and speed in 1- (1- chlorine cyclopropyl) ethyl ketone synthesis process, temperature during cyclization
Accurate rigorous control is obtained, the generation of by-product is reduced, reduces the generation of tar, improves the receipts of 1- (1- chlorine cyclopropyl) ethyl ketone
Rate substantially reduces synthesising reacting time.
A kind of method continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction provided by the present invention, packet
Include following steps:
S1, raw material a and catalyst are pumped into after the first mixing module 7 in micro passage reaction mixes simultaneously, are sent to the
One warm-up block 8 is preheated；
S2, the second warm-up block 9 that chloro- 2 pentanone of 3,5- bis- is pumped into micro passage reaction is preheated；
S3, through step S1 and step S2 preheating after substance simultaneously send to the second mixing module 10 of micro passage reaction into
Row hybrid concurrency gives birth to cyclization；
S4, the mixture through cyclization obtained by step S3 send the refrigerating module 11 to micro passage reaction to be cooled down；
S5, it collects through mixture cooling in step S4 and send to collecting tiered container 12 and be successively layered, extract, close
And organic phase, then dried with anhydrous sodium sulfate to get 1- (1- chlorine cyclopropyl) ethyl ketone is arrived；
Wherein, the raw material a in liquid alkaline, liquid potassium hydroxide, liquid potassium carbonate, liquid sodium carbonate one
Kind；
The micro passage reaction is mixed including the first mixing module 7, the first warm-up block 8, the second warm-up block 9, second
Mold block 10, refrigerating module 11, wherein the pipe outlet of the first mixing module 7 and the entrance of the first warm-up block 8 connect
It connects, the pipe outlet of the pipe outlet of the first warm-up block 8 and the second warm-up block 9 is connected to the second mixing module 10
Two entrance connections, the pipe outlet of the second mixing module 10 are connect with the entrance of refrigerating module 11；The cooling
The pipe outlet of module 11 is connected with the collection tiered container 12 outside micro passage reaction.
Preferably, the raw material a is 20% liquid alkaline.
Preferably, in the cyclization, 20% liquid alkaline, catalyst, chloro- 2 pentanone of 3,5- bis- feed intake mass ratio be 1:
0.25:2.2。
Preferably, first warm-up block 8, the second warm-up block 9, the temperature of material in the second mixing module 10
It is identical, it is 70 DEG C.
Preferably, the cooling temperature in the refrigerating module 11 is 20 DEG C.
Preferably, the catalyst is polyethylene glycol 400, tetra-n-butyl ammonium bromide, trimethyl n-octyl ammonium bromide.
Preferably, first warm-up block 8 and 9 preheating time of the second warm-up block are 2-5 minutes, the cooling mould
11 cooling time of block is 1-3 minutes.
Preferably, 7 incorporation time of the first mixing module is 1-3 minutes, 10 incorporation time of the second mixing module
It is 5-8 minutes.
It preferably, further include that Waste Heat Recovery recycles, specific steps are as follows:
Heat exchanger 13, heat exchanger are set between the second mixing module 10 and refrigerating module 11 of micro passage reaction
The heat that second mixing module 10 is carried out the mixture after cyclization by the cooling medium in 13 absorbs, after absorbing heat
Cooling medium import the first warm-up block 8, the second warm-up block 9, in the second mixing module 10.
Preferably, temperature of the mixture after 13 heat exchange of over-heat-exchanger after carrying out cyclization is 20 DEG C -40 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention utilizes multiple micro passage reactions, in the preparation process of 1- (1- chlorine cyclopropyl) ethyl ketone, raw material a
It mixes sufficiently and rapidly, then is carried out rapidly and after being uniformly preheating to required temperature with catalyst, and equally carried out rapidly and
The mixing module that chloro- 2 pentanone of 3,5- bis- of even preheating enters next stage carries out cyclization, because of the mixing of micro passage reaction
The large specific surface area of module is heated rapidly and uniform, is greatly shortened the time required to cyclization, it is only necessary to and 5-8 minutes, thus significantly
The hydrolysis for reducing 1- (1- chlorine cyclopropyl) ethyl ketone reduce the incidence of tar to reduce the production of by-product；
(2) in preferred embodiment of the invention, liquid alkaline concentration is preferably 20%, and the concentration of liquid alkaline is too small or is mostly unfavorable for very much
The synthesis of compound 1- (1- chlorine cyclopropyl) ethyl ketone, liquid alkaline concentration is too low, the cyclization and chloro thing of 3,5- bis- chloro- 2 pentanones
Hydrolysis formed competition, cause the yield of 1- (1- chlorine cyclopropyl) ethyl ketone lower；And the concentration of liquid alkaline it is higher when, side reaction
Increase, coking extent is serious, yield decline；
(3) in preferred embodiment of the invention, it is preferable that in the cyclization, 20% liquid alkaline, catalyst, 3,5- bis- are chloro-
2 pentanones feed intake mass ratio as 1:0.25:2.2, and the yield of this ratio, obtained 1- (1- chlorine cyclopropyl) ethyl ketone is
82.5%-92.9%；The catalytic efficiency of catalyst is optimal, 20% liquid alkaline and 3, and the ratio of chloro- 2 pentanone of 5- bis- is also to need strictly
Control, because the dosage of liquid alkaline is insufficient, with the progress of reaction, liquid alkaline is gradually consumed, when liquid alkaline in reaction solution
When quality is lower than certain value, the cyclization of the hydrolysis than chloro- 2 pentanone of 3,5- bis- of 1- (1- chlorine cyclopropyl) ethyl ketone will lead to
Fastly, it so liquid alkaline obtains quality accounting height and is conducive to cyclization, in addition also needs liquid alkaline dosage to be not easy too excess and causes to waste；
(4) in preferred embodiment of the invention, it is preferable that first warm-up block 8, the second warm-up block 9, second are mixed
The temperature for molding material in block 10 is 70 DEG C, and the temperature of reaction system is controlled at 70 DEG C, 1- (1- chlorine cyclopropyl) is conducive to
The generation of ethyl ketone；
(5) in preferred embodiment of the invention, it is preferable that temperature set by the refrigerating module 11 is 20 DEG C, will be anti-
Product 1- (1- chlorine cyclopropyl) ethyl ketone is answered to be rapidly cooled to 20 DEG C and carry out subsequent collection and hierarchical operations rapidly, it can be significantly
Reduction reaction product 1- (1- chlorine cyclopropyl) carry out reaction again and generate other by-products, and be conducive to 1- (1- chlorine cyclopropyl) second
Ketone is layered and isolated operation, and the scald of operator will not be caused in separation operation process；
(6) in preferred embodiment of the invention, it is preferable that 9 preheating time of first warm-up block 8 and the second warm-up block
It is 2-5 minutes, 11 cooling time of refrigerating module is 1-3 minutes, and strict control preheating time can reach 70 DEG C
Reaction is participated in, energy consumption is not wasted；Strict control cooling time, reaction product be cooled to 20 DEG C can carry out subsequent collection and point
Layer operation, the by-product reduced in reaction process generate；
(7) in preferred embodiment of the invention, it is preferable that the incorporation time that first mixing module 7 is set is 1-3 point
Clock, the incorporation time that second mixing module 10 is set is 5-8 minute, energy saving, and strict control is cyclized the time, avoids
The generation of the hydrolysis of product 1- (1- chlorine cyclopropyl) ethyl ketone；
(8) in preferred embodiment of the invention, it is preferable that in the second mixing module 10 and refrigerating module of micro passage reaction
Heat exchanger 13 is set between 11, and the cooling medium in heat exchanger 13 will be mixed after the second mixing module 10 progress cyclization
The heat for closing object is absorbed, and it is mixed that the cooling medium after absorbing heat imports the first warm-up block 8, the second warm-up block 9, second
Molding block 10 is recycled.Because needing to carry out cooling treatment before to the mixed collection and layered shaping after cyclization, lead to
Over-heat-exchanger is by the heat recovery of the mixture after cyclization and is sent into the first warm-up block 8, the second warm-up block 9, the
Two mixing modules 10 are recycled, and can reduce cost with saving heat energy；
(9) present invention prepares 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction, and preparation time is than traditional reaction kettle
Required time is greatly reduced, and is foreshortened within half an hour from 3,4 hours of traditional handicraft, and the energy is saved, and improves raw material
Conversion ratio and product yield, save the cost reduce the generation of by-product, decrease wastewater flow rate caused by production.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, come specifically with the embodiment of several different experiments effects of the invention below
It is bright.A specific embodiment of the invention is shown in detail by following embodiment.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes part of this application, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and do not constitute the improper restriction invented in fact this.In the accompanying drawings:
Fig. 1 is the process flow chart for preparing 1- (1- chlorine cyclopropyl) ethyl ketone of the invention；
Fig. 2 is the apparatus structure schematic diagram that 1- (1- chlorine cyclopropyl) ethyl ketone is prepared using micro passage reaction of the invention.
In figure: 1, raw material a holding vessel；2, the chloro- 2 pentanone holding vessel of 3,5- bis-；3, metering pump；4, metering pump；5, catalyst
Holding vessel；6, metering pump；7, the first mixing module；8, the second warm-up block；9, the second warm-up block；10, the second mixing module；
11, refrigerating module；12, tiered container is collected；13, heat exchanger.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
The present invention provides a kind of method for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction, referring to figure
1 process flow chart of the invention, this method includes the following steps: S1, by raw material a and catalyst while being pumped into microchannel plate and answers
After the first mixing module 7 in device, preheated into the first warm-up block 8；S2, chloro- 2 pentanone of raw material 3,5- bis- is pumped into it is micro-
The second warm-up block 9 in channel reactor is preheated；Substance after S3, above-mentioned steps S1 and step S2 are preheated enters simultaneously
Second mixing module 10 of micro passage reaction, the raw cyclization of hybrid concurrency；S4, cyclization mixture send to microchannel
The refrigerating module 11 of reactor is cooled down；Through overcooled reaction product in S5, collection step S4, layering is extracted, and is merged
Organic phase, then dried with anhydrous sodium sulfate to get required product 1- (1- chlorine cyclopropyl) ethyl ketone is arrived.
It further include that Waste Heat Recovery recycles, the specific steps are as follows: in microchannel plate in some preferred embodiments of the invention
Setting heat exchanger 13 is answered between the second mixing module 10 of device and refrigerating module 11, the cooling medium in heat exchanger 13 is by the
The heat that two mixing modules 10 carry out the mixture after cyclization is absorbed, and the cooling medium after absorbing heat imports first
Warm-up block 8, the second warm-up block 9, the second mixing module 10 are recycled.
It should be appreciated that the heat that heat exchanger 13 recycles can be used for the first warm-up block 8, the second warm-up block 9, the
The one of module or multiple modules of two mixing modules 10.
Below by embodiment, the invention will be further described, but content not thereby limiting the invention.
Embodiment 1
As shown in Fig. 2, controlling metering pump 3,6 so that 20% liquid alkaline is with the flow velocity of 1kg/h, catalyst tetra-n-butyl ammonium bromide
With 0.25m3The flow velocity of/h enters the first mixing module 7 of micro passage reaction, and the incorporation time of the first mixing module 7 is set as
Enter the first warm-up block 8 after 1 minute, mixing 1 minute, the set temperature of the first warm-up block 8 is 70 DEG C, preheating time 2
Minute；Metering pump 4 is controlled so that 3,5- bis- chloro- 2 pentanones enter the second warm-up block 9, the second pre- hot-die with the flow velocity of 2.2kg/h
The set temperature of block 9 is 70 DEG C, preheating time is 2 minutes；After preheating 2 minutes, by 20% and mixture, 3, the 5- bis- of catalyst
Chloro- 2 pentanone is passed through in the second mixing module 10 carries out cyclization simultaneously, and 10 set temperature of the second mixing module is 70 DEG C, mixes
Closing the reaction time is 5 minutes；After five minutes, the mixture of gained cyclization carries out waste heat through over-heat-exchanger 13 to cyclization
It recycles and recycles, the heat of the mixture of gained cyclization is absorbed through the cooling medium in heat exchanger 13, absorbs heat
Cooling medium afterwards carries out waste heat recycling in importing the first warm-up block 8；Cyclisation after heat exchanger 13 absorbs heat
The mixture temperature of reaction is 22 DEG C, enters back into refrigerating module 11, refrigerating module set temperature is 20 DEG C, cooling time is 1 point
Clock；It after 1 minute cooling, collect and is layered, water phase is extracted, and merges organic phase, then dry with anhydrous sodium sulfate, needed for obtaining
Product 1- (1- chlorine cyclopropyl) ethyl ketone, light yellow liquid, 3,5- bis- chloro- 2 pentanone conversion ratios 93.8%, 1- (1- chlorine cyclopropyl) second
Ketone yield is 87.2%.
Embodiment 2
As shown in Fig. 2, controlling metering pump 3,6 so that 20% liquid alkaline is with the flow velocity of 1kg/h, catalyst tetra-n-butyl ammonium bromide
With 0.25m3The flow velocity of/h enters the first mixing module 7 of micro passage reaction, and the incorporation time of the first mixing module 7 is set as
Enter the first warm-up block 8 after 3 minutes, mixing 3 minutes, the set temperature of the first warm-up block 8 is 70 DEG C, preheating time 5
Minute；Metering pump 4 is controlled so that 3,5- bis- chloro- 2 pentanones enter the second warm-up block 9, the second pre- hot-die with the flow velocity of 2.2kg/h
The set temperature of block 9 is 70 DEG C, preheating time is 5 minutes；It preheats after five minutes, by 20% and mixture, 3, the 5- bis- of catalyst
Chloro- 2 pentanone is passed through in the second mixing module 10 carries out cyclization simultaneously, and 10 set temperature of the second mixing module is 70 DEG C, mixes
Closing the reaction time is 8 minutes；After cyclization 8 minutes, the mixture of gained cyclization carries out waste heat through over-heat-exchanger 13
It recycles and recycles, the heat of the mixture of gained cyclization is absorbed through the cooling medium in heat exchanger 13, absorbs heat
Cooling medium afterwards carries out waste heat recycling in importing the first warm-up block 8；Cyclisation after heat exchanger 13 absorbs heat
The mixture temperature of reaction is 40 DEG C, enters back into refrigerating module 11, refrigerating module set temperature is 20 DEG C, cooling time is 3 points
Clock；It after 3 minutes cooling, collect and is layered, water phase is extracted, and merges organic phase, then dry with anhydrous sodium sulfate, needed for obtaining
Product 1- (1- chlorine cyclopropyl) ethyl ketone, light yellow liquid, 3,5- bis- chloro- 2 pentanone conversion ratios 96.2%, 1- (1- chlorine cyclopropyl) second
Ketone yield is 92.9%.
The reaction step of embodiment 3-10 is consistent with embodiment 2, raw material a, catalyst, chloro- 2 pentanone of 3,5- bis- feed ratio
Example is consistent with embodiment 2, when the preheating of the incorporation time of the first mixing module 7, the first warm-up block 8 and the second warm-up block 9
Between, the incorporation time of the second mixing module 10 is consistent with embodiment 2；Other different parameters and obtained conversion
Rate and yield are shown in Table one.
Table one
It is learnt by table one, in some schemes of the invention, raw material a is 20% liquid alkaline, 20% liquid alkaline, catalyst, 3,5- bis-
Chloro- 2 pentanone feeds intake mass ratio as 1:0.25:2.2, and the yield of 1- (1- chlorine cyclopropyl) ethyl ketone is 82.5%-92.9%.
Raw material a be 20% liquid alkaline, 20% liquid alkaline, catalyst, chloro- 2 pentanone of 3,5- bis- feed intake mass ratio be 1:0.25:2.2,
When cyclization temperature is 70 DEG C, cooling temperature is 20 DEG C, it is more advantageous to the cyclization of chloro- 2 pentanone of 3,5- bis-, 1- (1- chlorine
Cyclopropyl) ethyl ketone yield is best, substantially within the scope of 87.2%-92.9%.Comparative example 4 it is found that cyclisation temperature be 75 DEG C when, 1-
(1- chlorine cyclopropyl) ethyl ketone yield also reaches 87.1%, it is contemplated that the factor of saving heat energy, so cyclization temperature of the invention
Preferably 70 DEG C of degree.
It should be appreciated that the heat that above-described embodiment 1-10 is only recycled with heat exchanger 13 is for the first warm-up block 8
The elaboration that example is made.
More than, only presently preferred embodiments of the present invention is not intended to limit the present invention in any form；All current rows
The those of ordinary skill of industry can be shown in by specification attached drawing and above and swimmingly implement the present invention；But all to be familiar with sheet special
The technical staff of industry without departing from the scope of the present invention, is made a little using disclosed above technology contents
The equivalent variations of variation, modification and evolution is equivalent embodiment of the invention；Meanwhile all substantial technologicals according to the present invention
The variation, modification and evolution etc. of any equivalent variations to the above embodiments, still fall within technical solution of the present invention
Within protection scope.
Claims (10)
1. a kind of method for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction, which is characterized in that including with
Lower step:
After S1, the first mixing module (7) mixing for being pumped into raw material a and catalyst in micro passage reaction simultaneously, send to first
Warm-up block (8) is preheated；
S2, the second warm-up block (9) that chloro- 2 pentanone of 3,5- bis- is pumped into micro passage reaction is preheated；
S3, the substance after step S1 and step S2 preheating are sent simultaneously to the second mixing module (10) progress of micro passage reaction
Hybrid concurrency gives birth to cyclization；
S4, the mixture through cyclization obtained by step S3 send to the refrigerating module of micro passage reaction (11) and are cooled down；
S5, it collects through mixture cooling in step S4 and send to collecting tiered container (12) and be successively layered, extract, merge
Organic phase, then dried with anhydrous sodium sulfate to get 1- (1- chlorine cyclopropyl) ethyl ketone is arrived；
Wherein, the raw material a is selected from one of liquid alkaline, liquid potassium hydroxide, liquid potassium carbonate, liquid sodium carbonate；
The micro passage reaction includes the first mixing module (7), the first warm-up block (8), the second warm-up block (9), second
Mixing module (10), refrigerating module (11), wherein the pipe outlet of the first mixing module (7) and the pipe of the first warm-up block (8)
The connection of road entrance, the pipe outlet of the first warm-up block (8) and the pipe outlet of the second warm-up block (9) are connected to second
Two entrances of mixing module (10) connect, the pipe outlet of the second mixing module (10) and the pipeline of refrigerating module (11)
Entrance connection；The pipe outlet of the refrigerating module (11) is connected with the collection tiered container (12) outside micro passage reaction.
2. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that the raw material a is 20% liquid alkaline.
3. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 2
Method, which is characterized in that 20% liquid alkaline, catalyst, chloro- 2 pentanone of 3,5- bis- feed intake mass ratio as 1:0.25:2.2.
4. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that first warm-up block (8), the second warm-up block (9), the material in the second mixing module (10)
Temperature is identical, is 70 DEG C.
5. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that the cooling temperature in the refrigerating module (11) is 20 DEG C.
6. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that the catalyst is polyethylene glycol 400, tetra-n-butyl ammonium bromide, trimethyl n-octyl ammonium bromide.
7. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that first warm-up block (8) and the second warm-up block (9) preheating time are 2-5 minutes, the cooling
11 cooling time of module is 1-3 minutes.
8. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that the first mixing module (7) incorporation time is 1-3 minutes, and the second mixing module (10) cyclisation is anti-
It is 5-8 minutes between seasonable.
9. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 1
Method, which is characterized in that it further include that Waste Heat Recovery recycles, specific steps are as follows:
Heat exchanger (13) are set between the second mixing module (10) and refrigerating module (11) of micro passage reaction, heat exchange
The heat that mixing module (10) are carried out the mixture after cyclization by the cooling medium in device (13) absorbs, and absorbs heat
Rear cooling medium import the first warm-up block (8), the second warm-up block (9), in the second mixing module (10).
10. a kind of side for continuously preparing 1- (1- chlorine cyclopropyl) ethyl ketone using micro passage reaction according to claim 9
Method, which is characterized in that temperature of the mixture after the heat exchanger (13) heat exchange after cyclization is 20 DEG C -40
℃。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112079698A (en) * | 2020-09-27 | 2020-12-15 | 北京旭阳科技有限公司 | Process for preparing 1-chloro-1- (chloroacetyl) cyclopropane |
| CN117105759A (en) * | 2023-10-24 | 2023-11-24 | 江苏七洲绿色化工股份有限公司 | Method for continuously preparing 2-chloro-1- (1-chlorocyclopropyl) ethanone |
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