CN107098859A - A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol - Google Patents
A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol Download PDFInfo
- Publication number
- CN107098859A CN107098859A CN201710250679.3A CN201710250679A CN107098859A CN 107098859 A CN107098859 A CN 107098859A CN 201710250679 A CN201710250679 A CN 201710250679A CN 107098859 A CN107098859 A CN 107098859A
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- Prior art keywords
- kettle
- signal
- automatic control
- oxidation
- module
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D231/18—One oxygen or sulfur atom
- C07D231/20—One oxygen atom attached in position 3 or 5
- C07D231/22—One oxygen atom attached in position 3 or 5 with aryl radicals attached to ring nitrogen atoms
Abstract
The invention discloses a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol, synthesis system includes the oxidative system being sequentially connected, desolventizing system, water wash system and centrifugation systems；Synthesis system also includes sensor-based system and automatic control system, automatic control system and is connected respectively with oxidative system, desolventizing system, water wash system and centrifugation systems, and sensor-based system is connected with automatic control system, oxidative system and desolventizing 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 improved, while prevent toxic product from producing injury to the human body of the personnel of operation, therefore automaticity is higher.
Description
Technical field
The present invention relates to field of pesticide production, more particularly to a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol.
Background technology
Pyraclostrobin is new-type wide-spectrum bactericide.There is mitochondrial respiratory inhibitor protection, treatment, blade infiltration to pass
Lead effect.General to spray 3 times, interval 10d sprays 1 medicine.Number of times spray depending on the state of an illness.To cucumber, banana safety, poisoning is had no
Occur.
Pyrazoles alcohol for production pyraclostrobin intermediate in actual production functions of the equipments it is relatively simple, and can not be formed
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, simultaneously
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 is relatively low, and production needs substantial amounts of manpower again, therefore can cause to cause human body very big injury,
And production yield is not also high.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol, more
Plus environmental protection.
In order to realize above-mentioned technical purpose, the present invention is adopted the following technical scheme that：
A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol, synthesis system includes the oxidation system being sequentially connected
System, desolventizing system, water wash system and centrifugation systems；Synthesis system also includes sensor-based system and automatic control system, automatic control
System processed is connected with oxidative system, desolventizing system, water wash system and centrifugation systems respectively, and sensor-based system is respectively with automatically controlling
System, oxidative system are connected with desolventizing system；
Oxidative system includes stills for air blowing and oxidation feed arrangement, and desolventizing system includes precipitation kettle, condenser and solvent
Recovery tower, condenser is used to the DMF in precipitation kettle being cooled to liquids recovery in solvent recovery tower, and solvent recovery tower is used for
Reclaim the DMF of precipitation kettle separation；Water wash system includes washing kettle, and centrifugation systems include centrifuge and solvent groove；
The feed end of stills for air blowing is connected with aoxidizing the discharge end of feed arrangement by pipeline, the discharge end of precipitation kettle and washing
The feed end of kettle is connected also by pipeline, and the discharge end of washing kettle and the feed end of centrifuge are connected by pipeline, centrifuge
Discharge end is connected with the feed end of solvent groove also by pipeline, and dehvery pump and valve are set on the pipeline.
Further, if the sensor-based system, which includes, connects signal biography on dry temperature sensor, the temperature sensor
Defeated line, the signal transmssion line output end of the sensor-based system is connected with automatic control system, and the signal transmssion line of sensor-based system is defeated
Enter end to be connected with temperature sensor；
The automatic control system includes automatic controller and some signal transmssion lines；The automatic control system includes
The signal input module that is sequentially connected, signal amplification module, signal filtering module, signal analog-to-digital conversion module, signal of change with
Processing module, signal D/A converter module, output signal amplification module and signal output module；
The signal input module of the automatic control system is connected with some signal transmssion lines of sensor-based system respectively, institute
State signal output module by the signal transmssion line of automatic control system respectively with oxidative system, desolventizing system, water wash system and
Dehvery pump and the valve connection of centrifugation systems.
Further, the stills for air blowing include oxidation kettle, and the top side wall of the oxidation kettle sets feed end, institute
State oxidation kettle bottom and discharge end is set, the oxidation kettle top, which is set, is provided for stirring in motor, the stills for air blowing body
The puddler of material, the output end of the motor is connected by the top of shaft coupling and puddler, is laterally set on the puddler
Stirring cross bar is put, the two ends cutting ferrule of the stirring cross bar, the cutting ferrule sets stirring vertical rod by bearing, and stirring rod end is set
External gear is put, the oxidation inner wall of kettle sets ring gear, and external gear is engaged with ring gear.
Further, a pair of agitating plates are set in the stirring vertical rod.
Further, the cutting ferrule includes body, and body inwall sets some raised lines being evenly distributed, and the set is internal
Wall bottom be provided for holding drag bearing along plate.
The present invention technical characterstic and effect be：Produced using above-mentioned production line, improve the security performance of production,
Operation is more flexible, 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 improved, while preventing toxic product from producing injury, therefore oneself to the human body of the personnel of operation
Dynamicization degree is higher.
Brief description of the drawings
Fig. 1 is the structure chart of the present invention.
Fig. 2 is automatic control system flow chart of the present invention.
Fig. 3 is the structure chart of stills for air blowing of the present invention.
Fig. 4 is the sectional view of stills for air blowing of the present invention.
Fig. 5 is the sectional view of cutting ferrule of the present invention.
In figure：1 is oxidative system；2 be desolventizing system；3 be water wash system；4 be centrifugation systems；5 be sensor-based system；6 are
Automatic control system；7 be stills for air blowing；8 be oxidation feed arrangement；9 be precipitation kettle；10 be condenser；11 be solvent recovery tower；12
For washing kettle；13 be centrifuge；14 be solvent groove；15 be pipeline；16 be dehvery pump；17 be valve；18 be temperature sensor；
19 be signal transmssion line；20 be automatic controller；21 be signal input module；22 be signal amplification module；23 be signal filtering
Module；24 be signal analog-to-digital conversion module；25 be signal of change and processing module；26 be signal D/A converter module；27 be letter
Number output module；28 be oxidation kettle；29 be motor；30 be puddler；31 be stirring cross bar；32 be cutting ferrule；33 be bearing；34
For stirring vertical rod；35 be external gear；36 be ring gear；37 be agitating plate；38 be body；39 be raised line；40 be along plate；41 be defeated
Go out signal amplification module.
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 a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol, synthesis system bag
Include the oxidative system 1 being sequentially connected, desolventizing system 2, water wash system 3 and centrifugation systems 4；Synthesis system also includes sensing system
System 5 and automatic control system 6, automatic control system 6 respectively with oxidative system 1, desolventizing system 2, water wash system 3 and centrifugation systems
4 are connected, and sensor-based system 5 is connected with automatic control system 6, oxidative system 1 and desolventizing system 2 respectively；It can automatically control
The valve of said system and the switch of dehvery pump and closure, with can accurately transferring raw material and reaction in material.
Oxidative system 1 includes stills for air blowing 7 and oxidation feed arrangement 8, and desolventizing system 2 includes precipitation kettle 9, condenser 10
With solvent recovery tower 11, solvent recovery tower 11 is used for the DMF for reclaiming the separation of precipitation kettle 9；Water wash system 3 includes washing kettle 12,
Centrifugation systems 4 include centrifuge 13 and solvent groove 14；The discharge end of the feed end of stills for air blowing 7 and oxidation feed arrangement 8 leads to
Piping 15 is connected, and the discharge end of precipitation kettle 9 is connected with the feed end of washing kettle 12 also by pipeline 15, the discharging of washing kettle 12
End is connected with the feed end of centrifuge 13 by pipeline 15, the discharge end of centrifuge 13 and the feed end of solvent groove 14 also by
Pipeline 15 is connected, and dehvery pump 16 and valve 17 are set on pipeline 15.This apparatus system can be saved during material production
Transfer time, improve production efficiency.
If sensor-based system 5 includes connection signal transmssion line 19 on dry temperature sensor 18, temperature sensor 18；It is described to pass
The signal transmssion line output end of sensing system is connected with automatic control system, and signal transmssion line input and the temperature of sensor-based system are passed
Sensor is connected；Automatic control system 6 includes automatic controller 20 and some signal transmssion lines 19；Automatic control system 6 includes
The signal input module 21 that is sequentially connected, signal amplification module 22, signal filtering module 23, signal analog-to-digital conversion module 24, letter
Number calculate with processing module 25, signal D/A converter module 26, output signal amplification module 41 and signal output module 27；
The signal input module 21 of automatic control system 6 is connected with some signal transmssion lines 19 of sensor-based system 5 respectively,
Signal output module 27 is respectively with oxidative system 1, desolventizing system 2, washing by the signal transmssion line 19 of automatic control system 6
The dehvery pump 16 and valve 17 of system 3 and centrifugation systems 4 are connected.It can monitor and control in real time using this control mode to produce car
Between situation and production reaction process time monitoring, manpower can be saved, it is to avoid to the damage of workman caused by artificial control
Evil.
Stills for air blowing 7 include oxidation kettle 28, and the top side wall of oxidation kettle 28 sets feed end, oxidation kettle 28 bottom
Discharge end is set, and oxidation kettle 28 top sets the puddler 30 for being provided for stirring material in motor 29, oxidation kettle 28, electricity
The output end of machine 29 is connected by shaft coupling with the top of puddler 30, and stirring cross bar 31, stirring are laterally set on puddler 30
The two ends cutting ferrule 32 of cross bar 31, cutting ferrule 32 sets stirring vertical rod 34 by bearing 33, and stirring vertical rod 34 top sets external gear 35,
Aoxidize the inwall of kettle 28 and ring gear 36 is set, external gear 35 is engaged with ring gear 36.A pair of agitating plates are set in stirring vertical rod 34
37.Cutting ferrule 32 includes body 38, and the inwall of body 38 sets some raised lines 39 being evenly distributed, and the inwall bottom of body 38, which is set, to be used
In hold drag bearing 33 along plate 40.Set using the direction of rotation and stirring vertical rod of puddler by bearing activity so that stirring
The direction of rotation of bar and stirring vertical rod on the contrary, and be the rotation because puddler, drive the stirring external gear of rod end and interior
Gear ring engagement just causes the direction of rotation of puddler and stirring vertical rod on the contrary, the raised line set is used for the outer of further fixing bearing
Wall, along the outside for being provided for support bearing of plate.
Because the product production process of intermediate of the present invention is that 1- (4- chlorphenyls) pyrazolidine -3- ketone is put into reactor
It is interior, add solvent DMF and be passed through oxygen 5-6 hours, be incubated for 1 small time, oxidation reaction is transferred to precipitation kettle after terminating, evaporation is reclaimed
DMF, precipitation adds water after terminating washs centrifugation, and solid phase obtains light yellow solid 1- (4- chlorphenyls) -3- pyrazoles alcohol.Using above-mentioned production
Line is produced, and improves the security performance of production, and operation is more flexible, saves manpower, improves production efficiency, while
So that the material of reaction raw materials and intermediate product is more accurate, therefore improves the quality of product, while preventing toxic product
Injury is produced to the human body of the personnel of operation, therefore automaticity is higher.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
1. a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol, it is characterised in that：Synthesis system, which includes, to be sequentially connected
Oxidative system (1), desolventizing system (2), water wash system (3) and centrifugation systems (4)；Synthesis system also includes sensor-based system
(5) and automatic control system (6), automatic control system (6) respectively with oxidative system (1), desolventizing system (2), water wash system (3)
Be connected with centrifugation systems (4), sensor-based system (5) respectively with automatic control system (6), oxidative system (1) and desolventizing system (2)
It is connected；
Oxidative system (1) includes stills for air blowing (7) and oxidation feed arrangement (8), and desolventizing system (2) includes precipitation kettle (9), cold
Condenser (10) and solvent recovery tower (11), condenser (10) are used to the DMF in precipitation kettle (9) being cooled to liquids recovery to solvent
In recovery tower (11), solvent recovery tower (11) is used for the DMF for reclaiming precipitation kettle (9) separation；Water wash system (3) includes washing kettle
(12), centrifugation systems (4) include centrifuge (13) and solvent groove (14)；
The feed end of stills for air blowing (7) is connected by pipeline (15) with the discharge end of oxidation feed arrangement (8), and precipitation kettle (9) go out
Material end is connected with the feed end of washing kettle (12) also by pipeline (15), the discharge end of washing kettle (12) and entering for centrifuge (13)
Expect that end is connected by pipeline (15), the discharge end of centrifuge (13) connects with the feed end of solvent groove (14) also by pipeline (15)
Connect, dehvery pump (16) and valve (17) are set on the pipeline (15).
2. a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol as described in claim, it is characterised in that：It is described to pass
Sensing system (5) connects signal transmssion line (19) if including dry temperature sensor (18) on the temperature sensor (18), described
Signal transmssion line (19) output end of sensor-based system (5) is connected with automatic control system (6), the signal transmission of sensor-based system (5)
Line (19) input is connected with temperature sensor (18)；
The automatic control system (6) includes automatic controller (20) and some signal transmssion lines (19)；It is described to automatically control
System (6) includes the signal input module (21) being sequentially connected, signal amplification module (22), signal filtering 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
And signal output module (27) (41)；
Some signal transmssion lines of the signal input module (21) of the automatic control system (6) respectively with sensor-based system (5)
(19) be connected, the signal output module (27) by the signal transmssion lines (19) of automatic control system (6) respectively with oxidation
System (1), desolventizing system (2), dehvery pump (16) and valve (17) connection of water wash system (3) and centrifugation systems (4).
3. a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol as described in claim, it is characterised in that：The oxygen
Change kettle (7) and include oxidation kettle (28), the top side wall of the oxidation kettle (28) sets feed end, the oxidation kettle
(28) bottom sets discharge end, and oxidation kettle (28) top sets to set in motor (29), the oxidation kettle (28) and used
In the puddler (30) of stirring material, the output end of the motor (29) is connected by shaft coupling with the top of puddler (30),
Stirring cross bar (31), the two ends cutting ferrule (32) of the stirring cross bar (31), the cutting ferrule are laterally set on the puddler (30)
(32) stirring vertical rod (34) is set by bearing (33), stirring vertical rod (34) top sets external gear (35), the oxidation kettle
(28) inwall sets ring gear (36), and external gear (35) is engaged with ring gear (36).
4. a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol as described in claim, it is characterised in that：It is described to stir
Mix and a pair of agitating plates (37) are set in vertical rod (34).
5. a kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol as described in claim, it is characterised in that：The card
Set (32) includes body (38), and body (38) inwall sets some raised lines (39) being evenly distributed, body (38) inwall
Bottom be provided for holding drag bearing (33) along plate (40).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250679.3A CN107098859A (en) | 2017-04-17 | 2017-04-17 | A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250679.3A CN107098859A (en) | 2017-04-17 | 2017-04-17 | A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol |
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| CN107098859A true CN107098859A (en) | 2017-08-29 |
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| CN201710250679.3A Pending CN107098859A (en) | 2017-04-17 | 2017-04-17 | A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977405A (en) * | 2017-04-17 | 2017-07-25 | 安徽广信农化股份有限公司 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol |
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| CN104211641A (en) * | 2014-08-19 | 2014-12-17 | 山东康乔生物科技有限公司 | Synthetic technology for pyraclostrobin |
| CN104592117A (en) * | 2015-01-13 | 2015-05-06 | 安徽国星生物化学有限公司 | Synthesis method of pyraclostrobin |
| CN105177727A (en) * | 2015-11-04 | 2015-12-23 | 奎屯银力棉油机械有限公司 | Automatic unginned cotton treating device combining drying and impurity removing |
| CN105177728A (en) * | 2015-11-04 | 2015-12-23 | 奎屯银力棉油机械有限公司 | Seed cotton cleaner capable of automatically uniformly feeding cottons |
| CN105968048A (en) * | 2016-06-07 | 2016-09-28 | 四川福思达生物技术开发有限责任公司 | Method for synthesizing pyraclostrobin intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole |
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2017
- 2017-04-17 CN CN201710250679.3A patent/CN107098859A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211641A (en) * | 2014-08-19 | 2014-12-17 | 山东康乔生物科技有限公司 | Synthetic technology for pyraclostrobin |
| CN104592117A (en) * | 2015-01-13 | 2015-05-06 | 安徽国星生物化学有限公司 | Synthesis method of pyraclostrobin |
| CN105177727A (en) * | 2015-11-04 | 2015-12-23 | 奎屯银力棉油机械有限公司 | Automatic unginned cotton treating device combining drying and impurity removing |
| CN105177728A (en) * | 2015-11-04 | 2015-12-23 | 奎屯银力棉油机械有限公司 | Seed cotton cleaner capable of automatically uniformly feeding cottons |
| CN105968048A (en) * | 2016-06-07 | 2016-09-28 | 四川福思达生物技术开发有限责任公司 | Method for synthesizing pyraclostrobin intermediate 1-(4-chlorophenyl)-3-hydroxy-1-h-pyrazole |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977405A (en) * | 2017-04-17 | 2017-07-25 | 安徽广信农化股份有限公司 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol |
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Application publication date: 20170829 |