CN110194725A - A kind of device and method of the continuous autoclave production imines of modified - Google Patents
A kind of device and method of the continuous autoclave production imines of modified Download PDFInfo
- Publication number
- CN110194725A CN110194725A CN201810159808.2A CN201810159808A CN110194725A CN 110194725 A CN110194725 A CN 110194725A CN 201810159808 A CN201810159808 A CN 201810159808A CN 110194725 A CN110194725 A CN 110194725A
- Authority
- CN
- China
- Prior art keywords
- kettle
- reaction kettle
- imines
- negative reaction
- continuous
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 150000002466 imines Chemical class 0.000 title abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 136
- VCSZQCLSILBVOH-UHFFFAOYSA-N CCC1=C(C(=CC=C1)CN)N=C(C)COC Chemical class CCC1=C(C(=CC=C1)CN)N=C(C)COC VCSZQCLSILBVOH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- JJVKJJNCIILLRP-UHFFFAOYSA-N 2-ethyl-6-methylaniline Chemical compound CCC1=CC=CC(C)=C1N JJVKJJNCIILLRP-UHFFFAOYSA-N 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- -1 2- ethyl -6- aminomethyl phenyl Chemical group 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000012074 organic phase Substances 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- GFMWQBMQWUPGLF-UHFFFAOYSA-N 1-methoxypropan-2-imine Chemical class COCC(C)=N GFMWQBMQWUPGLF-UHFFFAOYSA-N 0.000 claims 1
- 230000001934 delay Effects 0.000 claims 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims 1
- 230000035484 reaction time Effects 0.000 abstract description 12
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 150000007522 mineralic acids Chemical class 0.000 description 5
- CUZLJOLBIRPEFB-UHFFFAOYSA-N 1-methoxypropan-2-one Chemical compound COCC(C)=O CUZLJOLBIRPEFB-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000003377 acid catalyst Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- ZLCSFXXPPANWQY-UHFFFAOYSA-N 3-ethyltoluene Chemical compound CCC1=CC=CC(C)=C1 ZLCSFXXPPANWQY-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- WVQBLGZPHOPPFO-LBPRGKRZSA-N (S)-metolachlor Chemical compound CCC1=CC=CC(C)=C1N([C@@H](C)COC)C(=O)CCl WVQBLGZPHOPPFO-LBPRGKRZSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- RITABKMTBQXRIU-UHFFFAOYSA-N CCC1=C(C(=CC=C1)CN)C(C(=N)C)OC Chemical class CCC1=C(C(=CC=C1)CN)C(C(=N)C)OC RITABKMTBQXRIU-UHFFFAOYSA-N 0.000 description 1
- 239000005617 S-Metolachlor Substances 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/02—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of compounds containing imino groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the method and devices of continuous autoclave production N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines (abbreviation imines).The device of continuous autoclave production imines of the invention includes more concatenated kettles, and each kettle is sequentially connected by overflow pipe, last is the accumulator still of normal pressure, remaining each kettle is negative reaction kettle, and condenser and continuous division box is respectively configured.The method of continuous autoclave production imines of the invention produces imines using the device of continuous autoclave production imines of the invention.The device and method of continuous autoclave production imines of the invention is suitable for large-scale production, saves manpower, easy to operate, shortens the reaction time, and product quality is easy to stable homogeneous.
Description
Technical field
The invention belongs to pesticide chemical production field, in particular to a kind of chemical pesticide process units.
Background technique
(N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines, is commonly called as imines, is a kind of important organic
Compound, in the synthesis process of Chiral pesticide S-metolachlor, imines is the key intermediate of synthesis of amine ethers.Traditional conjunction
Method at imines is mainly methoxy acetone and 2- methyl -6- ethyl-aniline route.One kind disclosed in CN101781230A
The method of synthesizing imine by catalytic dehydration, using iodine as catalyst, heating reflux reaction in the presence of azeotropy dehydrant, by amine and ketone
Condensation dehydration generates imines.A kind of method of acidic catalyst dehydration synthesis N- aryl ketimide disclosed in CN102898329A,
Using inorganic acid or solid acid as catalyst, heating reflux reaction in the presence of azeotropy dehydrant, by ketone and arylamine condensation production
N- aryl ketimide.
Above method mostly uses greatly batch process production, and ((N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- is sub-
Amine, although the conversion ratio of raw material is higher, it is longer to be needed the reaction time, the auxiliary operations holding time such as charging and discharging
It is longer, the loss of material and energy is easily caused, and complicated for operation, product quality is also difficult to keep stable.
Summary of the invention
In view of above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of continuous production ((N-
The process unit and production method of (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines
Provide that a kind of smooth operation simplicity, high degree of automation, the reaction time is shorter, consersion unit small volume, produces
The uniform continuous autoclave of quality produces (device of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines and side
Method.
Meanwhile production (the device of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines disclosed by the invention
It can be also used for the production of its similar substance.
Specific inventive technique scheme is as follows:
A kind of Chemical Manufacture (process unit of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines, spy
Sign is that the device includes 1 or 1 or more negative reaction kettle, in a series arrangement the normal pressure accumulator still with 1 or 1 or more
It is connected, normal pressure accumulator still is located at behind negative reaction kettle.
The process unit, it is characterised in that finally one or more is normal pressure accumulator still in each kettle, remaining is
Negative reaction kettle, and condenser and continuous division box is respectively configured；Each kettle is sequentially connected by overflow pipe.
The negative reaction kettle is 2 or more, and negative reaction kettle connects in a series arrangement；
Overflow port is provided on the negative reaction kettle, the overflow port is located at the 50%~90% of kettle body height, excellent
It selects at 75%~85% height；The overflow pipe is connected to the overflow port.
Guide shell is configured in the accumulator still and negative reaction kettle；
The maximum height that the liquid level that each negative reaction kettle is configured so that in each kettle can reach successively reduces；
The continuous division box is continuous valve tower.
Each kettle is stainless steel material；The condenser is stainless steel material, and the heat exchange area of condenser is 15m2~
100m2；The continuous division box is stainless steel material；The continuous valve tower is packed tower.
Reaction raw materials are pumped to First negative reaction kettle by flow, and stirring forms reaction solution, and then reaction solution is from the
Successively overflow is to subsequent negative reaction kettle for one negative reaction kettle, and up to last, then overflow, to normal pressure accumulator still, completion is anti-
It answers.
Device described above can be used in production (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines and
Its analog.
A kind of continuous autoclave production (method of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines, spy
Sign is, using device described in any one of Claims 1 to 44, as production (N- (2- ethyl -6- aminomethyl phenyl) -1- first
The device of oxygroup propane -2- imines；
Wherein, reaction raw materials are continuously added in the 1st negative reaction kettle, then make the mixing of the reaction raw materials
Object is condensed into liquid phase by condenser followed by each negative reaction kettle, the gas phase of the negative reaction kettle back flow reaction
Afterwards, moisture is continuously separated by the continuous valve tower, organic phase is back in reaction kettle；The last overflow of reaction mass is to normal pressure
Accumulator still completes reaction, obtains product.
The reaction raw materials are 2- methyl -6- ethyl aniline and methoxy acetone.
Each negative reaction kettle reaction temperature is 50-120 DEG C, and it is 0.01-1.0MPa that negative reaction kettle, which reacts vacuum degree,.
Invention effect
According to the present invention it is possible to provide a kind of smooth operation simplicity, high degree of automation, product quality uniform continuous kettle
Formula produces the (device and method of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines.Moreover, make us it is imaginary not
To using apparatus and method of the present invention production (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines
When, the reaction time is substantially reduced, the complete raw material of unreacted can be recycled by subsequent imines rectifying, not cause original
Material list consumes in increased situation, effectively reduces production cost.
The continuous autoclave production that the present invention uses be (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines
Method solves the defects of traditional intermittent reaction is complicated for operation, and the reaction time is long.The technology of the present invention is produced using successive reaction
Product, reaction raw materials arrive normal-pressure reaction kettle output since into First negative reaction kettle, and the residence time is about 8 hours, and
Continuous uninterrupted production.Compared to intermittent reaction production method, not only the reaction time is short, while not needing to stop industrial production.Greatly
The reaction time is shortened greatly, improves production efficiency.In addition, plural serial stage reactor synthesizes imines in the technology of the present invention
Continuous reaction smooth operation is easy, avoids operation that is frequent broken empty and vacuumizing, production technology advantage is clearly
Detailed description of the invention
Fig. 1 is the schematic diagram of an example of the preferred embodiment of the device of the invention.
1- steam inlet regulating valve, 2- continuous reaction apparatus, 3- guide shell, baffle, 4- feedstock flowmeter, 5- raw material
Feed regulating valve, 6- pressure transmitter, 7- temperature transmitter, 8- condenser, 9- valve tower, 10- overflow pipe, 11- vacuum point
Distribution tank, 12- accumulator still
The specific embodiment of invention
Hereinafter, producing (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines to continuous autoclave of the invention
Device and method be specifically described.It is emphasized that following embodiment is only used for that the content of present invention is explained further, side
Just those skilled in the art of the present technique understand, are not intended to limit protection scope of the present invention, and related personnel is obvious to the present invention
Change, still the present invention claims protection scope within.
Embodiment 1
Fig. 1 shows continuous autoclave production of the invention, and (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- is sub-
An example of the preferred embodiment of the device of amine.
Referring to Fig.1 it is found that in this embodiment, continuous autoclave of the invention produces (N- (2- ethyl -6- methylbenzene
Base) device of -1- methoxy propane -2- imines includes more concatenated kettles, and they are sequentially connected by overflow pipe, last
For normal pressure accumulator still, remaining each kettle is negative reaction kettle, and every negative reaction kettle configures a set of condenser and continuously divides water
Tower.It is provided with overflow port on each negative reaction kettle, the overflow pipe is connected to the overflow port.Each kettle configures
Guide shell.Each negative reaction autoclave body product can be arranged according to actual needs.The condenser and valve tower are negative pressure equipment,
It needs to set different size according to specific production.
The maximum height that the liquid level that each negative reaction kettle is configured so that in each kettle can reach successively reduces, and needs
It is noted that " maximum height that liquid level can reach " is usually exactly described for each negative reaction kettle
The position of overflow port, when the liquid level in kettle reaches the overflow port, liquid is flowed out from the overflow port, and the liquid level no longer rises
It is high.In general, institute can be arranged at 50%~90% (preferably 75%~85%) of the kettle body height of each negative reaction kettle
State overflow port, the maximum height that the liquid level in each kettle can reach successively reduce by 150~500mm (preferably 200~
300mm)。
Overflow pipe preferred angled slope installation between each kettle, can reduce the resistance of Flow of Goods and Materials.Each kettle
It is preferably provided with agitating device, the agitating device is preferably single layer press-down type agitating paddle.Agitating mode is preferably pusher stirring.
The agitating device is equipped with baffle, and baffle number is 2~4 pieces.
Reaction raw materials methoxy acetone, 2- methyl -6- ethyl-aniline, toluene, catalyst are continuously added to First negative pressure
In reaction kettle, each negative reaction kettle shares a set of vacuum system.The raw material can pass through feed flow meter and regulating valve
The regulation and control to feed rate is realized in combination, or sets specific feed rate by metering pump.For example, charging is adjusted
Valve can be the pneumatic control valve chain with feed rate, and the feed flow meter of the raw material can set connection to scale
Lock control.
Each negative reaction kettle is preferably provided with external jacket, is passed through heat medium, realizes the heating to material in kettle.Heating
Medium entrance is preferably provided with pneumatic control valve, for adjusting the flow or pressure of heat medium.Temperature instrumentation is equipped in kettle, preferably
Temperature transmitter passes through the automatic control with the chain realization temperature in the kettle of heat medium import pneumatic control valve, it is ensured that technique
Safety and stability.Each negative reaction kettle is equipped with pressure instrumentation, preferably pressure transmitter, it is ensured that pressure meets work in kettle
Skill requirement.
The normal pressure accumulator still is preferably provided with external jacket, is passed through cooling medium, realizes the cooling to material in kettle.It is set in kettle
There are temperature instrumentation, preferable temperature transmitter.Pressure instrumentation, preferably pressure transmitter are equipped in kettle.
The feed pipe of the reaction raw materials be preferably inserted into liquid level in guide shell hereinafter, and density it is small reaction raw materials it is closeer
It is deeper to spend big reaction raw materials insertion depth, material stroke can be prevented short-circuit, guarantee that material comes into full contact with.
Material is using the potential difference between each kettle followed by each more concatenated negative pressure in the negative reaction kettle
Reaction kettle, the gas phase mixture of the interior abjection of kettle separate water by the continuous valve tower after the condenser is condensed into liquid phase
Point, to be synthesized the (reaction of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines.Reaction product is through most
In latter negative reaction kettle continuous overflow to normal pressure accumulator still, into normal pressure system, product is produced after the reaction was completed.
Embodiment 2
Reaction unit includes five negative reaction kettles and a normal pressure accumulator still, reaction raw materials --- methoxy acetone/first
Benzene liquid, 2- methyl -6- ethyl-aniline, inorganic acid catalyst are measured by flowmeter respectively with 1000L/h, 320L/h, 0.3L/h
Flow be pumped to First negative reaction kettle, reaction solution from First negative reaction kettle overflow to second, and so on it is straight
To the 5th, each negative reaction kettle is kept stirring speed in 260~300rpm.Pressure reaction still volume is 5000L, reaction temperature
80 DEG C of degree, reaction pressure (vacuum degree) are 0.075MPa.
Whole process, reaction raw materials --- methoxy acetone/toluene liquid, 2- methyl -6- ethyl-aniline, inorganic acid catalysis
Agent continuous feed by a certain percentage is reacted, reaction solution continuous discharge, keeps entire reaction continuous at vacuum degree 0.075MPa
It carries out.Reaction process temperature is stablized, and input and output material is continuous, successive reaction 8h.No. 5 negative reaction kettle reaction solution outlets measure 2- first
Base -6- ethyl-aniline conversion is 81%.
Due to the technology of the present invention using successive reaction produce product, reaction raw materials since into First negative reaction kettle,
To normal-pressure reaction kettle output, the residence time is about 8 hours, and continuous uninterrupted production.Compared to intermittent reaction production method, no
Only the reaction time is short (intermittent reflection generally needs about 24 hours from being dosed into output), while not needing to stop industrial production.
In contrast, successive reaction greatly shortens the reaction time, improves the utilization rate of equipment.
Embodiment 3
Reaction unit includes six negative reaction kettles and a normal pressure accumulator still, reaction raw materials --- methoxy acetone/first
Benzene liquid, 2- methyl -6- ethyl-aniline, inorganic acid catalyst are measured by flowmeter respectively with 1500L/h, 480L/h, 0.5L/h
Flow be pumped to First negative reaction kettle, reaction solution from First negative reaction kettle overflow to second, and so on it is straight
To the 6th, finally from the 6th negative reaction kettle overflow to accumulator still, into normal pressure system.Each negative reaction kettle is kept stirring
Speed is in 260~300rpm.Pressure reaction still volume is 6300L, and 80 DEG C of reaction temperature, reaction pressure (vacuum degree) is
A set of condenser and continuous valve tower is respectively configured in 0.075MPa, 1~No. 6 reaction kettle.
Whole process, methoxy acetone/toluene liquid, 2- methyl -6- ethyl-aniline, inorganic acid catalyst press certain ratio
Example continuous feed reaction, reaction solution continuous discharge keep entire reaction to be carried out continuously at vacuum degree 0.075MPa.Reaction process
Temperature is stablized, and input and output material is continuous, successive reaction 8h.No. 6 negative reaction kettle reaction solution outlets measure 2- methyl -6- ethyl-aniline
Conversion ratio is 82%.
Reaction raw materials discharge since into First negative reaction kettle to from the 5th negative reaction kettle, the residence time about 8
Hour.Intermittent reaction accounts for the kettle time (containing auxiliary time of production) about 24 hours, and in contrast, successive reaction greatly shortens
Reaction time improves the utilization rate of equipment.
The continuous autoclave production that the present invention uses be (N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines
Method and technology advantage is clearly:
Firstly, solving the defects of traditional intermittent reaction is complicated for operation, and the reaction time is long.
Secondly, the plural serial stage reactor makes imines synthesis continuous reaction smooth operation easy, avoid frequent
Operation that is broken empty and vacuumizing, greatly improves the degree of automation of process flow.
In addition most surprisingly, producing (N- (2- ethyl -6- methylbenzene using apparatus and method of the present invention
Base) -1- methoxy propane -2- imines when, effectively shorten the reaction time.
Finally, by the method for the invention, the complete raw material of unreacted can be recycled by subsequent imines rectifying, do not having
It causes to effectively reduce production cost in the increased situation of raw material consumption.
Claims (10)
1. a kind of Chemical Manufacture (process unit of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines, feature
It is that the device includes 1 or 1 or more negative reaction kettle, in a series arrangement the normal pressure accumulator still phase with 1 or 1 or more
Connection, normal pressure accumulator still are located at behind negative reaction kettle.
2. process unit according to claim 1, it is characterised in that last one or more delays in each kettle for normal pressure
Water rushes kettle, remaining is negative reaction kettle, and condenser and continuous division box is respectively configured；
Each kettle is sequentially connected by overflow pipe.
3. process unit according to claim 1, it is characterised in that the negative reaction kettle is 2 or more, negative reaction
Kettle connects in a series arrangement；
Overflow port is provided on the negative reaction kettle, the overflow port is located at the 50%~90% of kettle body height, preferably
At 75%~85% height；
The overflow pipe is connected to the overflow port.
4. process unit according to claim 1, it is characterised in that configuration is led in the accumulator still and negative reaction kettle
Flow cartridge；
The maximum height that the liquid level that each negative reaction kettle is configured so that in each kettle can reach successively reduces；
The continuous division box is continuous valve tower.
5. process unit according to any one of claims 1 to 4, wherein each kettle is stainless steel material；
The condenser is stainless steel material, and the heat exchange area of condenser is 15m2~100m2；
The continuous division box is stainless steel material；
The continuous valve tower is packed tower.
6. according to process unit according to any one of claims 1 to 4, it is characterised in that reaction raw materials pass through flow pump
Send to First negative reaction kettle, stirring forms reaction solution, then reaction solution from First negative reaction kettle successively overflow to rear
Continuous negative reaction kettle, until last, then overflow, to normal pressure accumulator still, completion is reacted.
7. process unit according to any one of claims 1 to 4, it is characterised in that described device is for producing (N- (2-
Ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines and the like.
8. a kind of continuous autoclave produces (method of N- (2- ethyl -6- aminomethyl phenyl) -1- methoxy propane -2- imines, feature
It is, using process unit described in any one of Claims 1 to 44, as production (N- (2- ethyl -6- aminomethyl phenyl) -1-
The device of methoxy propane -2- imines；
Wherein, reaction raw materials are continuously added in the 1st negative reaction kettle, then make the mixture of the reaction raw materials according to
It is secondary to flow through each negative reaction kettle, the gas phase of the negative reaction kettle back flow reaction after condenser is condensed into liquid phase,
Moisture is continuously separated by the continuous valve tower, organic phase is back in reaction kettle；
The last overflow of reaction mass completes reaction, obtains product to normal pressure accumulator still.
9. according to the method described in claim 8, it is characterized in that, the reaction raw materials are 2- methyl -6- ethyl aniline and first
Oxygroup acetone.
10. according to the method described in claim 8, it is characterized in that, each negative reaction kettle reaction temperature be 50-120 DEG C,
It is 0.01-1.0MPa that negative reaction kettle, which reacts vacuum degree,.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810159808.2A CN110194725A (en) | 2018-02-26 | 2018-02-26 | A kind of device and method of the continuous autoclave production imines of modified |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810159808.2A CN110194725A (en) | 2018-02-26 | 2018-02-26 | A kind of device and method of the continuous autoclave production imines of modified |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110194725A true CN110194725A (en) | 2019-09-03 |
Family
ID=67750759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810159808.2A Pending CN110194725A (en) | 2018-02-26 | 2018-02-26 | A kind of device and method of the continuous autoclave production imines of modified |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110194725A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112500391A (en) * | 2020-12-14 | 2021-03-16 | 江西禾益化工股份有限公司 | Device and method for producing dithianon through continuous kettle type reaction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0556297A1 (en) * | 1990-11-05 | 1993-08-25 | Exxon Chemical Patents Inc | Process for producing imines and/or amines from alcohols. |
| CN104803875A (en) * | 2015-03-27 | 2015-07-29 | 江苏长青农化南通有限公司 | Synthetic method for S-metolachlor |
| CN107537423A (en) * | 2017-08-09 | 2018-01-05 | 凯莱英生命科学技术(天津)有限公司 | Continuous still reaction device and n-BuLi participate in the continuous still reaction system of production |
-
2018
- 2018-02-26 CN CN201810159808.2A patent/CN110194725A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0556297A1 (en) * | 1990-11-05 | 1993-08-25 | Exxon Chemical Patents Inc | Process for producing imines and/or amines from alcohols. |
| CN104803875A (en) * | 2015-03-27 | 2015-07-29 | 江苏长青农化南通有限公司 | Synthetic method for S-metolachlor |
| CN107537423A (en) * | 2017-08-09 | 2018-01-05 | 凯莱英生命科学技术(天津)有限公司 | Continuous still reaction device and n-BuLi participate in the continuous still reaction system of production |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112500391A (en) * | 2020-12-14 | 2021-03-16 | 江西禾益化工股份有限公司 | Device and method for producing dithianon through continuous kettle type reaction |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102491905A (en) | Method and device for co-production of o-phenylenediamine and p-phenylenediamine | |
| CN116063363B (en) | Process for synthesizing emamectin benzoate intermediate by using intermittent microchannel reactor | |
| CN106631694B (en) | A kind of preparation method of 2,2,3,3- tetrafluoropropanol | |
| CN110194725A (en) | A kind of device and method of the continuous autoclave production imines of modified | |
| CN111589394A (en) | Ultrasonic homogeneous single-tube reactor | |
| CN201746485U (en) | Apparatus of preparing m-phenol diamine by continuous hydrolysis of metaphenylene diamine | |
| CN103724370B (en) | The processing method of phosphite ester compound is prepared in the coupling of a kind of reactive distillation | |
| CN209010417U (en) | A kind of device of the continuous autoclave production imines of modified | |
| CN103102369B (en) | A kind of production method of diethyl ethylphosphate | |
| CN102190602B (en) | Method and equipment for preparing phenyl carbamate through continuous reaction | |
| CN102294204B (en) | Integrated system technology of fixed bed and injection floating bed coupled with separating unit | |
| CN111302904A (en) | Alkylation continuous reaction device for BHT production | |
| CN210009939U (en) | Device for converting diethyl carbonate into ethyl methyl carbonate | |
| CN216630748U (en) | Production device of high-purity phenylacetic acid ethyl ester | |
| CN208244724U (en) | A kind of pantolactone synthesis reactor | |
| CN217410727U (en) | Device for continuously producing 2-methyl-3-methoxybenzoic acid | |
| CN110813207A (en) | Continuous channel reactor for synthesizing acrylate resin, polymerization reaction device and application | |
| CN102397772A (en) | High-efficient reation kettle | |
| CN215611599U (en) | Reaction system for continuously producing tromethamine | |
| CN109611668A (en) | A kind of reaction unit of band heat dissipation damping | |
| CN213699889U (en) | Tubular reactor | |
| CN102127228B (en) | Production process for synthesizing methyl vinyl silicone rubber | |
| CN103497323A (en) | Synthetic method for methoxy polyoxyethylene ether (methyl) acrylate | |
| CN106984061A (en) | Continuous countercurrent extraction process and equipment for 1, 5-pentanediamine | |
| CN113150021A (en) | Method for synthesizing boron trifluoride complex by using microchannel reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190903 |
|
| RJ01 | Rejection of invention patent application after publication |