CN106977405A - The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol - Google Patents
The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol Download PDFInfo
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- CN106977405A CN106977405A CN201710250680.6A CN201710250680A CN106977405A CN 106977405 A CN106977405 A CN 106977405A CN 201710250680 A CN201710250680 A CN 201710250680A CN 106977405 A CN106977405 A CN 106977405A
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- pipeline
- kettle
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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
Abstract
The invention discloses the synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol, synthesis system includes the esterification system set gradually, nitrification, hydrolysis system, centrifugation systems, sensor-based system and automatic control system, sensor-based system is connected with esterification system, nitrification, hydrolysis system and automatic control system respectively, and automatic control system is connected with esterification system, nitrification, hydrolysis 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 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 the synthesis system of field of pesticide production, more particularly to Yi Zhong Evil humulone Intermediate nitro phenol.
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
A variety of annual unifacial leaves and broadleaf weed are prevented and kill off, is mainly used in paddy field weed-killer, to the peanut of dry land, cotton, sugarcane etc. also
Effectively.
The intermediate of nitrophenol Wei Sheng Chan Evil humulones functions of the equipments in actual production are relatively simple, and can not form life
Producing 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, produce simultaneously
The raw material and intermediate of product production or some accessory substances are readily volatilized, cause to produce poison gas in workshop, and due to existing
Some production automation degrees are relatively low, and production needs substantial amounts of manpower again, therefore can cause to cause human body very big injury, and
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 phenol, more
Environmental protection.
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 phenol, synthesis system include set gradually esterification system,
Nitrification, hydrolysis system, centrifugation systems, sensor-based system and automatic control system, sensor-based system respectively with esterification system, nitrification
System, hydrolysis system are connected with automatic control system, and automatic control system is respectively with esterification system, nitrification, hydrolysis
System, centrifugation systems are connected with sensor-based system；
If the sensor-based system includes connects signal transmssion line on dry temperature sensor, the temperature sensor；It is described
Automatic control system includes signal input module, signal amplification module, signal filtering module, the signal analog-to-digital conversion being 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 transmssion line output end of sensor-based system is connected with the signal input module of automatic control system；
Esterification system includes esterifying kettle, and nitrification includes nitrating pot, and hydrolysis system includes hydrolysis kettle, centrifugation system
System includes centrifugation kettle and solvent receiving slit, and the discharge end of esterifying kettle and the feed end of nitrating pot are connected by pipeline, nitrating pot
Discharge end and the feed end of hydrolysis kettle connected by pipeline, the feed end of the discharge end and centrifugation kettle of the hydrolysis kettle passes through pipe
Road is connected, and the discharge end of centrifugation kettle 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 esterifying kettle sets motor, and the output end of the motor is set by shaft coupling to be stirred
Bar, the puddler is located in esterifying kettle, and the top of esterifying kettle sets first charging aperture and second charging aperture, first charging
First feed arrangement is set on mouthful, and the first feed arrangement includes feed hopper, and the bottom of the feed hopper sets the first pipeline A,
First pipeline A bottom connection metering ball, the bottom of the metering ball sets the first pipeline B, the bottom of the first pipeline B with
First charging aperture is connected；Esterification system also includes head tank, and the bottom of head tank is set sets second on discharging opening, discharging opening
Pipeline, discharge end connection the second pipe A and second pipe B, second pipe A of second pipe discharge end connects with second charging aperture
Connect, the discharge end of the second pipe B is connected with the first pipeline A.
Further, the connectivity part of the first pipeline A and feed hopper sets switch valve, the first pipeline B, second pipe A
Dehvery pump is set on switch valve, second pipe with all being set on second pipe B.
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, while the feeding device set causes charging more to facilitate accurate and save space, further improves
Production efficiency and conversion rate of products.
Brief description of the drawings
Fig. 1 is the structural system figure of the present 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 esterifying kettle of the present invention.
In figure：1 is esterification system；2 be nitrification；3 be hydrolysis system；4 be centrifugation systems；5 be sensor-based system；6 are
Automatic control system；7 be esterifying kettle；8 be nitrating pot；9 be hydrolysis kettle；10 be centrifugation kettle；11 be solvent receiving slit；12 be electricity
Machine；13 be puddler；14 be first charging aperture；15 be second charging aperture；16 be pipeline；17 be dehvery pump；18 be TEMP
Device；19 be signal transmssion line；20 be switch valve；21 be signal input module；22 be signal amplification module；23 be signal filtering mould
Block；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 signal
Output module；28 be output signal amplification module；29 be the first feed arrangement；30 be feed hopper；31 be the first pipeline A；32 are
Measure ball；33 be the first pipeline B；34 be head tank；35 be discharging opening；36 be second pipe；37 be second pipe A；38 be
Two pipeline B.
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. 1-4 are refer to, the present invention provides the synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol, it is characterised in that：
Synthesis system include the esterification system 1 set gradually, nitrification 2, hydrolysis system 3, centrifugation systems 4, sensor-based system 5 and from
Autocontrol system 6, sensor-based system 5 is connected with esterification system 1, nitrification 2, hydrolysis system 3 and automatic control system 6 respectively
Connect, automatic control system 6 is connected with esterification system 1, nitrification 2, hydrolysis system 3, centrifugation systems 4 and sensor-based system 5 respectively
Connect；If sensor-based system 5 includes connection signal transmssion line 19 on dry temperature sensor 18, temperature sensor 18；Automatically control and be
System 6 includes the signal input module 21 being sequentially connected, signal amplification module 22, signal filtering module 23, signal modulus modulus of conversion
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；Esterification system
System 1 includes esterifying kettle 7, and nitrification 2 includes nitrating pot 8, and hydrolysis system 3 includes hydrolysis kettle 9, and centrifugation systems 4 include
There are centrifugation kettle 10 and solvent receiving slit 11, the discharge end of esterifying kettle 7 is connected with the feed end of nitrating pot 8 by pipeline 16, nitrify
The discharge end of kettle 8 is connected with the feed end of hydrolysis kettle 9 by pipeline 16, the feed end of the discharge end and centrifugation kettle 10 of hydrolysis kettle 9
Connected by pipeline 16, the discharge end of centrifugation kettle 10 is connected with the feed end of solvent receiving slit 11 by pipeline 16, on pipeline 16
Dehvery pump 17 and switch valve 20 are set.The valve of said system and the switch of dehvery pump and closure can be automatically controlled, with can
Material in accurate transferring raw material and reaction, the transfer time that this apparatus system can be saved during material production, is improved
Production efficiency.Therefore save the space of device, improve production efficiency and conversion ratio, i.e., can using this control mode
The time monitoring of the process of the situation and production reaction of monitoring in real time and control workshop, can save manpower, it is to avoid artificial
Infringement caused by control to workman.
The top of esterifying kettle 7 sets motor 12, and the output end of motor 12 sets puddler 13, puddler 13 by shaft coupling
In esterifying kettle 7, the top of esterifying kettle 7 is set to be set in first charging aperture 14 and second charging aperture 15, first charging aperture 14
First feed arrangement 29, the first feed arrangement 29 includes feed hopper 30, and the bottom of feed hopper 30 sets the first pipeline A31, the
One pipeline A31 bottom connection metering ball 32, metering ball 32 bottom set the first pipeline B33, the first pipeline B33 bottom with
First charging aperture 14 is connected；Esterification system 1 also includes head tank 34, and the bottom of head tank 34 sets discharging opening 35, discharging opening
Second pipe 36, discharge end connection the second pipe A37 and second pipe B38, second pipe A37 of second pipe 36 are set on 35
Discharge end be connected with second charging aperture 15, second pipe B38 discharge end is connected with the first pipeline A31.First pipeline A31
Set all to set on switch valve 20, the first pipeline B33, second pipe A37 and second pipe B38 with the connectivity part of feed hopper 30 and open
Close and dehvery pump 17 is set on valve 20, second pipe 36.All set out using this feeding manner, and in the upper and lower side of metering ball
Valve is closed, the material quantity into esterifying kettle can be calculated, and is that liquids are calculated using volume calculation, i.e. spheroid volume
The volume of material, and then the quality of material is calculated, while the set-up mode of the above-mentioned pipeline set is in order to by the material in feed hopper
Quantitatively be added in esterifying kettle, then the liquid material added into esterifying kettle in feed pipe is also possible to as water, can clean into
Residual material in hopper, so enables to the proportioning of reaction mass more accurate, and the reaction accuracy for improving material is also carried
The conversion ratio of high material.
Because the product production process of intermediate of the present invention is that the chlorophenesic acid of metering and catalyst are put into esterifying kettle, drop
Plus POCl3, after reaction completely, room temperature is cooled to, esterified material is put into nitrating pot, stirring is cooled to 0~5 DEG C；Start drop
Plus nitration mixture, after reaction completely, it is cooled to 10 DEG C or so；Material in nitrating pot is gone into hydrolysis kettle, starts that process water is added dropwise, is added dropwise
End is cooled to 0~10 DEG C, and stirs centrifuge is discharged to after 1h, adds appropriate process water rinsing solid material, produces
Nitrophenol.Produced using above-mentioned production line, improve the security performance of production, operation is more flexible, saves manpower,
Production efficiency is improved, while also make it that the material of reaction raw materials and intermediate product is more accurate, therefore product is improved
Quality, while prevent toxic product from producing injury to the human body of the personnel of operation, therefore automaticity is higher, while set
Feeding device causes charging more to facilitate accurate and save space, further improves production efficiency and conversion rate of products.
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 (3)
1. the synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol, it is characterised in that：Synthesis system includes what is set gradually
Esterification system (1), nitrification (2), hydrolysis system (3), centrifugation systems (4), sensor-based system (5) and automatic control system (6),
Sensor-based system (5) is connected with esterification system (1), nitrification (2), hydrolysis system (3) and automatic control system (6) respectively,
Automatic control system (6) respectively with esterification system (1), nitrification (2), hydrolysis system (3), centrifugation systems (4) and sensing be
System (5) 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) includes the signal input module (21) being sequentially connected, 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 with the signal input module (21) of automatic control system (6) to be connected；
Esterification system (1) includes esterifying kettle (7), and nitrification (2) includes nitrating pot (8), and hydrolysis system (3) includes water
Kettle (9) is solved, centrifugation systems (4) include centrifugation kettle (10) and solvent receiving slit (11), the discharge end and nitrating pot of esterifying kettle (7)
(8) feed end is connected by pipeline (16), and the discharge end of nitrating pot (8) passes through pipeline (16) with the feed end of hydrolysis kettle (9)
Connection, the discharge end of the hydrolysis kettle (9) is connected with the feed end of centrifugation kettle (10) by pipeline (16), centrifuges going out for kettle (10)
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 phenol as described in claim 1, it is characterised in that：The esterification
The top of kettle (7) sets motor (12), and the output end of the motor (12) sets puddler (13), the stirring by shaft coupling
Bar (13) is located in esterifying kettle (7), and the top of esterifying kettle (7) sets first charging aperture (14) and second charging aperture (15), described
First feed arrangement (29) is set in first charging aperture (14), and the first feed arrangement (29) includes feed hopper (30), it is described enter
The bottom of hopper (30) sets the first pipeline A (31), the first pipeline A (31) bottom connection metering ball (32), the metering ball
(32) bottom sets the first pipeline B (33), and the bottom of the first pipeline B (33) is connected with first charging aperture (14)；Esterification
System (1) also includes head tank (34), and the bottom of head tank (34) sets discharging opening (35), and discharging opening sets second on (35)
Pipeline (36), the discharge end connection second pipe A (37) and second pipe B (38) of second pipe (36), second pipe A's (37)
Discharge end is connected with second charging aperture (15), and the discharge end of the second pipe B (38) is connected with the first pipeline A (31).
3. the synthesis system of the Yi Zhong Evil humulone Intermediate nitro phenol as described in claim 2, it is characterised in that：First pipeline
A (31) and feed hopper (30) connectivity part set switch valve (20), the first pipeline B (33), second pipe A (37) and second
All set on pipeline B (38) and dehvery pump (17) is set on switch valve (20), second pipe (36).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250680.6A CN106977405A (en) | 2017-04-17 | 2017-04-17 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250680.6A CN106977405A (en) | 2017-04-17 | 2017-04-17 | The synthesis system of Yi Zhong Evil humulone Intermediate nitro phenol |
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|---|---|---|---|---|
| US4420478A (en) * | 1978-04-14 | 1983-12-13 | Roussel Uclaf | Novel oximes |
| CN1566074A (en) * | 2003-06-13 | 2005-01-19 | 上海子能高科股份有限公司 | 4-methyl-3-nitrophenols and preparation method thereof |
| CN101823971A (en) * | 2010-03-16 | 2010-09-08 | 安徽科立华化工有限公司 | Synthesis method of 2,4-dichloro-5-isopropoxy aniline |
| CN102363597A (en) * | 2010-10-22 | 2012-02-29 | 连云港市金囤农化有限公司 | Preparation method of 2,4-dichloro-5-isopropoxy aniline salt |
| CN103880772A (en) * | 2014-04-08 | 2014-06-25 | 连云港市金囤农化有限公司 | Preparation method of oxadiargyl |
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-
2017
- 2017-04-17 CN CN201710250680.6A patent/CN106977405A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4420478A (en) * | 1978-04-14 | 1983-12-13 | Roussel Uclaf | Novel oximes |
| CN1566074A (en) * | 2003-06-13 | 2005-01-19 | 上海子能高科股份有限公司 | 4-methyl-3-nitrophenols and preparation method thereof |
| CN101823971A (en) * | 2010-03-16 | 2010-09-08 | 安徽科立华化工有限公司 | Synthesis method of 2,4-dichloro-5-isopropoxy aniline |
| CN102363597A (en) * | 2010-10-22 | 2012-02-29 | 连云港市金囤农化有限公司 | Preparation method of 2,4-dichloro-5-isopropoxy aniline salt |
| CN103880772A (en) * | 2014-04-08 | 2014-06-25 | 连云港市金囤农化有限公司 | Preparation method of oxadiargyl |
| CN107098859A (en) * | 2017-04-17 | 2017-08-29 | 安徽广信农化股份有限公司 | A kind of synthesis system of pyraclostrobin intermediate pyrazole alcohol |
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| 陆阳等: "新型高效除草剂氟胺草酯的合成", 《化工技术与开发》 * |
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Application publication date: 20170725 |