CN106905164A - The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers - Google Patents
The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers Download PDFInfo
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- CN106905164A CN106905164A CN201710250395.4A CN201710250395A CN106905164A CN 106905164 A CN106905164 A CN 106905164A CN 201710250395 A CN201710250395 A CN 201710250395A CN 106905164 A CN106905164 A CN 106905164A
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- Prior art keywords
- etherification
- kettle
- condenser
- signal
- cooling device
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention discloses the synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers, synthesis system includes dissolution system, etherification system, condenser system, centrifugation systems, sensor-based system and the automatic control system for setting gradually, sensor-based system is connected with dissolution system, etherification system, condenser system and automatic control system respectively, and automatic control system is connected with dissolution system, etherification system, condenser system, centrifugation systems and sensor-based system respectively.The present invention improves the security performance of production, operation is more flexible, save manpower, improve production efficiency, also cause that the material of reaction raw materials and intermediate product is more accurate simultaneously, therefore the quality of product is improve, while prevent the human body of personnel of the toxic product to operating from producing injury, therefore automaticity is higher.
Description
Technical field
The present invention relates to field of pesticide production, more particularly to Yi Zhong Evil humulone Intermediate nitro ethers synthesis system.
Background technology
【Alias】Agriculture thinks it；The 5- tert-butyl groups -3- (the chloro- 5- o-phenyl-isopropyls of 2,4- bis-) -1,3,4- oxadiazoline -2- ketone；
Evil humulone missible oil；Its missible oil is thought in agriculture；5- tertiary butyls -3- (the chloro- 5- o-phenyl-isopropyls of 2,4- bis-) -1,3,4- oxadiazoline -2- ketone；
Oxadiazon；5- tertiary butyls -3- (the chloro- 5- o-phenyl-isopropyls of 2,4- bis-)-quinoline -2- ketone；White crystals, odorless is non-hygroscopic；For
Various annual unifacial leaves and broadleaf weed are prevented and kill off, is mainly used in paddy field weed-killer, peanut, cotton, sugarcane to dry land etc. are also
Effectively.
The intermediate of nitro-ether Wei Sheng Chan Evil humulones functions of the equipments in actual production are relatively simple, and can not form production
Line, so production just waste the time of production, and the not accurate enough of reacting dose can be produced during using means of delivery, while product
The raw material and intermediate or some accessory substances of production are readily volatilized, cause to produce poison gas in workshop, and due to existing
Production automation degree it is relatively low, production needs substantial amounts of manpower again, therefore can cause to cause human body very big injury, and raw
Produce yield also not high.
The content of the invention
In order to solve the above technical problems, the present invention provides the synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers, more ring
Protect.
In order to realize above-mentioned technical purpose, the present invention is adopted the following technical scheme that：
The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers, synthesis system includes dissolution system, the ether for setting gradually
Change system, condenser system, centrifugation systems, sensor-based system and automatic control system, sensor-based system respectively with dissolution system, etherificate system
System, condenser system be connected with automatic control system, automatic control system respectively with dissolution system, etherification system, condenser system,
Centrifugation systems are connected with sensor-based system；
If the sensor-based system includes dry temperature sensor, signal transmssion line is connected on the temperature sensor；It is described
Automatic control system includes the signal input module, signal amplification module, signal filtering module, the signal analog-to-digital conversion that are sequentially connected
Module, signal of change and processing module, signal D/A converter module, output signal amplification module and signal output module；It is described
The signal transmission line output terminal of sensor-based system is connected with the signal input module of automatic control system；
Dissolution system includes dissolution kettle, and etherification system includes etherification kettle, and condenser system includes condenser, centrifugation system
System includes centrifugation kettle and solvent receiving slit, and the discharge end of dissolution kettle is connected with the feed end of etherification kettle by pipeline, etherification kettle
Discharge end be connected by pipeline with the feed end of condenser, the feed end of the discharge end of the condenser and centrifugation kettle is by pipe
Road is connected, and the discharge end that kettle is centrifuged is connected with the feed end of solvent receiving slit by pipeline, and dehvery pump and switch are set on pipeline
Valve.
Further, the top of the etherification kettle sets motor, and the output end of the motor is set by shaft coupling and stirred
Bar, the puddler is located in etherification kettle；It is horizontally disposed with-individual cooling device in etherification kettle, the cooling device of etherification kettle is from upper
Lower interval is equal, and cooling device is horizontally disposed snakelike cooling device, and puddler passes through the middle part of the cooling device of etherification kettle,
Horizontal puddler is set between adjacent two cooling device on puddler.
Further, cooling device includes steam-coil and spiral coil cooling tube, the outer wall of the steam-coil with
Spiral coil cooling tube is disposed proximate to.
Technical characterstic of the invention and effect are：Produced using above-mentioned production line, improve the security performance of production,
Operation more flexibly, saves manpower, improves production efficiency, while also causing the material of reaction raw materials and intermediate product more
Plus it is accurate, therefore the quality of product is improve, while prevent the human body of personnel of the toxic product to operating from producing injury, therefore certainly
Dynamicization degree is higher, while the feeding device for setting causes that charging more facilitates accurate and save space, further improves
Production efficiency and conversion rate of products.
Brief description of the drawings
Fig. 1 is structural system figure of the invention.
Fig. 2 is automatic control system flow chart of the present invention.
Fig. 3 is system diagram of the invention.
Fig. 4 is the sectional view of etherification kettle of the present invention.
Fig. 5 is the top view of cooling device.
In figure：1 is dissolution system；2 is etherification system；3 is condenser system；4 is centrifugation systems；5 is sensor-based system；6 are
Automatic control system；7 is dissolution kettle；8 is etherification kettle；9 is condenser；10 is centrifugation kettle；11 is solvent receiving slit；12 is electricity
Machine；13 is puddler；14 is cooling device；15 is steam-coil；16 is pipeline；17 is dehvery pump；18 is temperature sensor；
19 is signal transmssion line；20 is switch valve；21 is signal input module；22 is signal amplification module；23 is signal filtering module；
24 is signal analog-to-digital conversion module；25 is signal of change and processing module；26 is signal D/A converter module；27 is signal output
Module；28 is output signal amplification module；29 is spiral coil cooling tube.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Fig. 1-5 are refer to, the present invention provides the synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers, and synthesis system is included
Dissolution system 1, etherification system 2, condenser system 3, centrifugation systems 4, sensor-based system 5 and the automatic control system 6 for setting gradually, pass
Sensing system 5 is connected with dissolution system 1, etherification system 2, condenser system 3 and automatic control system 6 respectively, automatic control system 6
It is connected with dissolution system 1, etherification system 2, condenser system 3, centrifugation systems 4 and sensor-based system 5 respectively；
If sensor-based system 5 includes dry temperature sensor 18, signal transmssion line 19 is connected on temperature sensor 18；Automatic control
System processed 6 includes that the signal input module 21 being sequentially connected, signal amplification module 22, signal filtering module 23, signal modulus turn
Mold changing block 24, signal of change and processing module 25, signal D/A converter module 26, output signal amplification module 28 and signal output
Module 27；The output end of signal transmssion line 19 of sensor-based system 5 is connected with the signal input module 21 of automatic control system 6；
Dissolution system 1 includes dissolution kettle 7, and etherification system 2 includes etherification kettle 8, and condenser system 3 includes condenser 9,
Centrifugation systems 4 include centrifugation kettle 10 and solvent receiving slit 11, and the discharge end of dissolution kettle 7 is with the feed end of etherification kettle 8 by pipe
Road 16 is connected, and the discharge end of etherification kettle 8 is connected with the feed end of condenser 9 by pipeline 16, discharge end and the centrifugation of condenser 9
The feed end of kettle 10 is connected by pipeline 16, and the discharge end that kettle 10 is centrifuged is connected with the feed end of solvent receiving slit 11 by pipeline 16
Connect, dehvery pump 17 and switch valve 20 are set on pipeline 16.Can automatically control said system valve and dehvery pump switch and
Closure, with material that can accurately in transferring raw material and reaction, this apparatus system can save during material production turn
Shift time, improves production efficiency.Therefore the space of device is saved, production efficiency and conversion ratio is improve, i.e., using this
Control mode can monitor in real time and control workshop situation and production reaction process time monitoring, people can be saved
Power, it is to avoid the infringement caused by artificial control to workman.
The top of etherification kettle 8 sets motor 12, and the output end of motor 12 sets puddler 13, puddler 13 by shaft coupling
In etherification kettle 8；Be horizontally disposed with 2-3 cooling device 14 in etherification kettle 8, the cooling device 14 of etherification kettle 8 from top to bottom between
Every equal, cooling device 14 is horizontally disposed snakelike cooling device 14, and puddler 13 is through the cooling device 14 of etherification kettle 8
Middle part, is located at setting horizontal puddler 30 between adjacent two cooling device 14 on puddler 13.Cooling device 14 includes snakelike
Steam pipe 15 and spiral coil cooling tube 29, outer wall and the spiral coil cooling tube 29 of steam-coil 15 are disposed proximate to.Steam pipe and cooling
Pipe is disposed proximate to be to adjust suitable temperature rapidly while being cooled down after etherificate or being heated, and set in etherification kettle be also for
Rapid cooling or rapid cooling, while when to material carrying out cold filtration after esterification, existing due to setting cooling tube
In kettle, therefore chilling temperature is uneven, cause cooling pipe outer wall can residual solids particle, influence the quality of material and accurate
Degree, thus set close to heating tube can be to the residual of cooled and solidified material particles of somewhat being heated up around cooling pipe outer wall.Together
When the snakelike adjacent outer wall that constitutes of snakelike cooling or heater between have certain cavity, therefore facilitate puddler to hang down
Straight cutting enters the middle part of horizontally disposed snakelike device.And the puddler for setting can cause that material stirring is more uniform, can enter again
One step prevents the particle residue of cooling on the outside of snakelike tube wall.
Because the product production process of intermediate of the present invention is, by nitrophenol input dissolution kettle, to be transferred to appropriate dimethyl
Formamide, is discharged to etherification kettle, adds appropriate potassium carbonate, is warming up to 60 DEG C, starts that isopropyl bromide is added dropwise, and after completion of dropwise addition, delays
It is slow to be cooled to room temperature, then centrifuge separation is discharged to, obtain final product isopropyl ether.Produced using above-mentioned production line, improve life
The security performance of product, operation more flexibly, save manpower, improve production efficiency, while also cause reaction raw materials and in
Between product material it is more accurate, therefore the quality of product is improve, while preventing the human body of personnel of the toxic product to operating
Injury is produced, therefore automaticity is higher, while the feeding device for setting causes that charging more facilitates accurate and save space,
Further improve production efficiency and conversion rate of products.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (3)
1. the synthesis system of Yi Zhong Evil humulones Intermediate nitro ether, it is characterised in that：Synthesis system includes set gradually molten
Solution system (1), etherification system (2), condenser system (3), centrifugation systems (4), sensor-based system (5) and automatic control system (6), pass
Sensing system (5) is connected with dissolution system (1), etherification system (2), condenser system (3) and automatic control system (6) respectively, from
Autocontrol system (6) respectively with dissolution system (1), etherification system (2), condenser system (3), centrifugation systems (4) and sensor-based system
(5) it is connected；
The sensor-based system (5) connects signal transmission if including dry temperature sensor (18) on the temperature sensor (18)
Line (19)；The automatic control system (6) including be sequentially connected signal input module (21), signal amplification module (22), letter
Number filtration module (23), signal analog-to-digital conversion module (24), signal of change and processing module (25), signal D/A converter module
(26), output signal amplification module (28) and signal output module (27)；The signal transmssion line (19) of the sensor-based system (5) is defeated
Go out end to be connected with the signal input module (21) of automatic control system (6)；
Dissolution system (1) includes dissolution kettle (7), and etherification system (2) includes etherification kettle (8), and condenser system (3) includes cold
Condenser (9), centrifugation systems (4) include centrifugation kettle (10) and solvent receiving slit (11), the discharge end and etherification kettle of dissolution kettle (7)
(8) feed end is connected by pipeline (16), and the discharge end of etherification kettle (8) passes through pipeline (16) with the feed end of condenser (9)
Connection, the discharge end of the condenser (9) is connected with the feed end of centrifugation kettle (10) by pipeline (16), and going out for kettle (10) is centrifuged
Material end is connected with the feed end of solvent receiving slit (11) by pipeline (16), and dehvery pump (17) and switch valve are set on pipeline (16)
(20)。
2. the synthesis system of the Yi Zhong Evil humulone Intermediate nitro ethers as described in claim 1, it is characterised in that：The etherification kettle
(8) top sets motor (12), and the output end of the motor (12) sets puddler (13), the puddler by shaft coupling
(13) in etherification kettle (8)；2-3 cooling device (14), the cooling device of etherification kettle (8) are horizontally disposed with etherification kettle (8)
(14) it is spaced from top to bottom equal, cooling device (14) is horizontally disposed snakelike cooling device (14), and puddler (13) is passed through
The middle part of the cooling device (14) of etherification kettle (8), setting is horizontal between adjacent two cooling device (14) is located on puddler (13)
Puddler (30).
3. the synthesis system of the Yi Zhong Evil humulone Intermediate nitro ethers as described in claim 2, it is characterised in that：Cooling device
(14) steam-coil (15) and spiral coil cooling tube (29), the outer wall and spiral coil cooling tube of the steam-coil (15) are included
(29) it is disposed proximate to.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250395.4A CN106905164A (en) | 2017-04-17 | 2017-04-17 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250395.4A CN106905164A (en) | 2017-04-17 | 2017-04-17 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers |
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| Publication Number | Publication Date |
|---|---|
| CN106905164A true CN106905164A (en) | 2017-06-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710250395.4A Pending CN106905164A (en) | 2017-04-17 | 2017-04-17 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro ethers |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3836539A (en) * | 1971-09-09 | 1974-09-17 | Rhone Poulenc Sa | Oxadiazolone derivatives |
| CN101935282A (en) * | 2010-08-19 | 2011-01-05 | 合肥星宇化学有限责任公司 | Synthesis method of 1, 5-dichloro-2-iso propyl-4-nitrobenzene |
| CN106336385A (en) * | 2016-08-25 | 2017-01-18 | 江苏丰华化学工业有限公司 | Oxadiazon synthesis method |
-
2017
- 2017-04-17 CN CN201710250395.4A patent/CN106905164A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3836539A (en) * | 1971-09-09 | 1974-09-17 | Rhone Poulenc Sa | Oxadiazolone derivatives |
| CN101935282A (en) * | 2010-08-19 | 2011-01-05 | 合肥星宇化学有限责任公司 | Synthesis method of 1, 5-dichloro-2-iso propyl-4-nitrobenzene |
| CN106336385A (en) * | 2016-08-25 | 2017-01-18 | 江苏丰华化学工业有限公司 | Oxadiazon synthesis method |
Non-Patent Citations (1)
| Title |
|---|
| 冯景文: "《电气自动化工程》", 31 August 2016 * |
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Application publication date: 20170630 |