CN207091325U - A kind of hexazinone process units - Google Patents
A kind of hexazinone process units Download PDFInfo
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- CN207091325U CN207091325U CN201720772280.7U CN201720772280U CN207091325U CN 207091325 U CN207091325 U CN 207091325U CN 201720772280 U CN201720772280 U CN 201720772280U CN 207091325 U CN207091325 U CN 207091325U
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- kettle
- toluene
- pipeline
- hexazinone
- filter
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Abstract
The utility model discloses a kind of hexazinone process units, including the addition device being sequentially connected by pipeline, cyclization device and after-treatment device, addition device includes the addition kettle being sequentially communicated by pipeline and prepares kettle, prepare kettle and be provided with preparation kettle refluxing toluene mouth, prepare the outlet of kettle toluene and prepare kettle material outlet, cyclization device includes the first filter and ring-closure reaction device being sequentially communicated by pipeline, first filter prepares kettle material outlet by pipeline communication, after-treatment device includes the neutralization washing kettle being sequentially communicated by pipeline, precipitation kettle, crystallization kettle, second filter and products pot, prepare the outlet of kettle toluene, ring-closure reaction device and precipitation kettle pass through pipeline communication toluene dehydrating kettle.The utility model is easy to use, product yield is high, and the recycling to multi-solvents effectively reduces production cost.
Description
Technical field
It the utility model is related to hexazinone production technical field, and in particular to a kind of hexazinone process units.
Background technology
Hexazinone is interior suction selective herbicide, and plant roots, leaf can absorb, mainly be conducted by xylem, to pine tree
Root is not injured, and is excellent woods herbicide.In the production process of hexazinone, substantial amounts of toluene, petroleum ether have been used
Equal solvent, toluene belong to poisonous chemical, there is certain harm to environment and human body, so can not directly discharge, and pass through
The hexazinone product yield that traditional hexazinone production technology obtains is low, and production cost is high, in consideration of it, being necessary to use hexazinone
Process units makes improvements.
The content of the invention
To solve the deficiencies in the prior art, the purpose of this utility model be to provide it is a kind of it is easy to use, product yield is high,
And the recycling to multi-solvents effectively reduces the hexazinone process units of production cost.
In order to realize above-mentioned target, the utility model adopts the following technical scheme that：
A kind of hexazinone process units, including addition device, cyclization device and the post processing being sequentially connected by pipeline
Device, addition device include the addition kettle being sequentially communicated along Flow of Goods and Materials direction by pipeline and prepare kettle, prepare kettle and be provided with
Kettle refluxing toluene mouth is prepared, prepare the outlet of kettle toluene and prepares kettle material outlet, cyclization device includes leading to along Flow of Goods and Materials direction
The first filter and ring-closure reaction device that piping is sequentially communicated, the first filter are prepared kettle material by pipeline communication and gone out
Mouthful, neutralization washing kettle that after-treatment device includes being sequentially communicated by pipeline along Flow of Goods and Materials direction, precipitation kettle, crystallization kettle, the
Two filters and products pot, the second filter also connect filtrate by pipeline and handle kettle, and the outlet of preparation kettle toluene, cyclization are anti-
Answer device and precipitation kettle by pipeline communication toluene dehydrating kettle.
Preferably, foregoing toluene dehydrating kettle is connected by pipeline communication toluene tank, toluene tank by the first return line
Logical addition kettle.
More preferably, foregoing filtrate processing kettle is provided with aqueous phase outlet and organic phase outlet.
It is highly preferred that foregoing aqueous phase outlet passes through in pipeline communication and extraction kettle, neutralize extraction kettle and pass through the second return duct
Kettle refluxing toluene mouth is prepared in road connection.
It is further preferred that foregoing organic phase outlet passes through the 3rd return line by pipeline communication distillation still, distillation still
Connect precipitation kettle.
Specifically, foregoing toluene dehydrating kettle, neutralization washing kettle, neutralization extraction kettle pass through pipeline communication wastewater disposal basin.
Preferably, foregoing first filter and distillation still pass through pipeline communication waste residue pond.
More preferably, drying device is also connected with by pipeline between foregoing second filter and products pot.
It is of the present utility model to be beneficial in that：Easy to use, the product of hexazinone process units of the present utility model
Yield is high, and toluene can be effectively reclaimed by toluene dehydrating kettle, and can be sent into addition kettle and recycle, the toluene reclaimed through distillation still
It can also be sent into precipitation kettle and recycle with petroleum ether mixed solvent, the organic phase of neutralized extraction kettle recovery, which can be sent into, to be prepared in kettle
Recycle, the recycling to multi-solvents effectively reduces production cost.
Brief description of the drawings
Fig. 1 is work connection diagram of the present utility model.
Embodiment
Make specific introduce to the utility model below in conjunction with the drawings and specific embodiments.
Referring to Fig. 1, a kind of hexazinone process units of the present embodiment, including the addition being sequentially connected by pipeline fill
Put, cyclization device and after-treatment device.
Addition device includes the addition kettle being sequentially communicated along Flow of Goods and Materials direction by pipeline and prepares kettle, prepares and is set on kettle
Have and prepare kettle refluxing toluene mouth, prepare the outlet of kettle toluene and prepare kettle material outlet, toluene dehydrating kettle passes through pipeline communication toluene
Storage tank, toluene tank connect addition kettle by the first return line.
Cyclization device includes the first filter and ring-closure reaction device being sequentially communicated along Flow of Goods and Materials direction by pipeline,
First filter prepares kettle material outlet by pipeline communication.
After-treatment device includes the neutralization washing kettle, precipitation kettle, crystallization being sequentially communicated along Flow of Goods and Materials direction by pipeline
Kettle, the second filter and products pot, also drying device is connected between the second filter and products pot by pipeline.Second
Filter also connects filtrate by pipeline and handles kettle, and filtrate processing kettle is provided with aqueous phase outlet and organic phase outlet, aqueous phase go out
Mouth in pipeline communication by, with extraction kettle, neutralizing extraction kettle and passing through the second return line connection preparation kettle refluxing toluene mouth；It is organic
Mutually outlet passes through pipeline communication distillation still, and distillation still connects precipitation kettle by the 3rd return line.
The outlet of kettle toluene, ring-closure reaction device and precipitation kettle are prepared by pipeline communication toluene dehydrating kettle, toluene dehydrating kettle,
Neutralize washing kettle, neutralization extraction kettle passes through pipeline communication wastewater disposal basin（It is not shown）, the first filter and distillation still pass through
Pipeline communication waste residue pond（It is not shown）, caused waste water and waste residue in production process, which are focused on, can avoid polluting environment.
In order to preferably illustrate the utility model, its course of work is specifically described below：
（1）Addition
A certain amount of toluene and methyl propylhomoserin ester are added in addition kettle, addition kettle chuck is passed through steam and is warming up to 50 DEG C
When, stopping is passed through steam and is passed through cooling water after vapour more than discharging, and a certain amount of cyclohexyl isocyanate is then slowly added dropwise and carries out
Addition reaction, controlling reaction temperature are 65 DEG C, and reaction pressure is normal pressure.
After addition reaction terminates, material is transferred to preparation kettle in kettle, after adding a certain amount of toluene, prepares kettle chuck and is passed through steaming
Vapour heats up, and negative pressure removes part toluene at 60 DEG C, and the toluene of abjection removes toluene dehydrating kettle, the reuse after 120 DEG C of normal pressures are dehydrated
In addition kettle, waste water removes wastewater disposal basin；Prepare leftover materials in kettle and obtain { [(cyclohexyl ammonia after the filtering of the first filter
Base) carbonyl] imino group } (dimethylamino) Ethyl formate（Intermediate I）Toluene solution it is stand-by, filter residue goes to waste residue pond.
（2）Cyclization
The toluene solution of intermediate I and methanol solution of sodium methylate are pumped into ring-closure reaction simultaneously with flow according to a certain percentage
In device, ring-closure reaction device chuck is passed through steam heating, and it is 65 DEG C to control cyclization reaction temperature, and reaction pressure is negative pressure, and side is reacted
Side negative pressure steams the ethanol of toluene, methanol and reaction generation, and the mixture that will be collected into（Toluene, methanol, ethanol）Send toluene
Dehydrating kettle, dewater treatment is carried out in 120 DEG C, normal pressure, waste water removes wastewater disposal basin.
（3）Post processing
The feed liquid obtained after the completion of ring-closure reaction is transferred to neutralization washing kettle, add a certain amount of acetic acid adjust to pH 7 ~
8, a certain amount of water washing, stratification are added, aqueous phase removes wastewater disposal basin, and organic phase is transferred to precipitation kettle, in 120 DEG C of vacuum distillations
Go out toluene, send toluene dehydrating kettle to be dehydrated in 120 DEG C of normal pressures；In precipitation kettle leftover materials through cooling water temperature to 80 DEG C when, add
After the mixed solution dilution of a certain amount of petroleum ether and toluene, crystallization kettle is transferred to, 5 DEG C are cooled to through ethylene glycol freezing liquid
Crystallization, then filtered through the second filter, filter cake send pan dryer to obtain hexazinone product after 60 DEG C, negative pressure drying.
Filtrate in second filter is transferred to filtrate processing kettle, adds a certain amount of hydrochloric acid and adjusts to pH3, stands and divide
Layer, upper organic phase 90 ~ 120 DEG C of air-distillations in distillation still, the toluene and petroleum ether mixed solvent of recovery are sent into precipitation kettle
In reuse, bottoms be sent into slag case；Lower floor's aqueous phase is transferred to neutralization extraction kettle, adds a certain amount of liquid caustic soda and adjusts to pH 7
After ~ 8, through toluene extracting and demixing, extraction organic phase, which is entered to prepare in kettle, to be reused, and aqueous phase extracted removes wastewater disposal basin.
The easy to use of hexazinone process units of the present utility model, product yield are high, can have by toluene dehydrating kettle
Effect recovery toluene, and can be sent into addition kettle and recycle, toluene and petroleum ether mixed solvent through distillation still recovery can be also sent into
Recycled in precipitation kettle, the organic phase of neutralized extraction kettle recovery can be sent into prepare to be recycled in kettle, the recovery to multi-solvents
Using effectively reducing production cost.
In description of the present utility model, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", " under ",
The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer " are
Based on orientation shown in the drawings or position relationship, it is for only for ease of description the utility model and simplifies description, rather than instruction
Or imply that signified device or element must have specific orientation, with specific azimuth configuration and operation, therefore be not understood that
For to limitation of the present utility model.In addition, term " first ", " second " be only used for describe purpose, and it is not intended that instruction or
Imply relative importance.
, it is necessary to which explanation, unless otherwise clearly defined and limited, term " are pacified in description of the present utility model
Dress ", " connected ", " connection " should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integratedly
Connection；Can be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary,
It can be the connection of two element internals.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition
Concrete meaning of the language in the utility model.
General principle, principal character and advantage of the present utility model has been shown and described above.The technical staff of the industry
It should be appreciated that above-described embodiment does not limit the utility model in any form, it is all by the way of equivalent substitution or equivalent transformation
The technical scheme obtained, all falls within the scope of protection of the utility model.
Claims (8)
1. a kind of hexazinone process units, it is characterised in that including addition device, the cyclization device being sequentially connected by pipeline
And after-treatment device, the addition device include the addition kettle being sequentially communicated along Flow of Goods and Materials direction by pipeline and prepare kettle,
The preparation kettle, which is provided with, to be prepared kettle refluxing toluene mouth, prepare the outlet of kettle toluene and prepares kettle material outlet, the cyclization device
Including the first filter and ring-closure reaction device being sequentially communicated along Flow of Goods and Materials direction by pipeline, the first filter passes through
Pipeline communication prepares kettle material outlet, and the after-treatment device includes the neutralization being sequentially communicated along Flow of Goods and Materials direction by pipeline
Washing kettle, precipitation kettle, crystallization kettle, the second filter and products pot, second filter also connect filtrate by pipeline
Kettle is handled, the outlet of preparation kettle toluene, ring-closure reaction device and the precipitation kettle pass through pipeline communication toluene dehydrating kettle.
2. a kind of hexazinone process units according to claim 1, it is characterised in that the toluene dehydrating kettle passes through pipe
Road connects toluene tank, and the toluene tank connects addition kettle by the first return line.
3. a kind of hexazinone process units according to claim 1, it is characterised in that the filtrate processing kettle is provided with
Aqueous phase exports and organic phase outlet.
4. a kind of hexazinone process units according to claim 3, it is characterised in that the aqueous phase outlet passes through pipeline
Connection neutralizes extraction kettle, and the neutralization extraction kettle is connected by the second return line prepares kettle refluxing toluene mouth.
5. a kind of hexazinone process units according to claim 3, it is characterised in that the organic phase outlet passes through pipe
Road connects distillation still, and the distillation still connects precipitation kettle by the 3rd return line.
6. a kind of hexazinone process units according to claim 4, it is characterised in that the toluene dehydrating kettle, neutralize
Washing kettle, neutralization extraction kettle pass through pipeline communication wastewater disposal basin.
7. a kind of hexazinone process units according to claim 5, it is characterised in that first filter and steaming
Kettle is evaporated by pipeline communication waste residue pond.
8. a kind of hexazinone process units according to claim 1, it is characterised in that second filter and production
Drying device is also connected with by pipeline between product tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720772280.7U CN207091325U (en) | 2017-06-29 | 2017-06-29 | A kind of hexazinone process units |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720772280.7U CN207091325U (en) | 2017-06-29 | 2017-06-29 | A kind of hexazinone process units |
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| Publication Number | Publication Date |
|---|---|
| CN207091325U true CN207091325U (en) | 2018-03-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201720772280.7U Active CN207091325U (en) | 2017-06-29 | 2017-06-29 | A kind of hexazinone process units |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433758A (en) * | 2019-08-23 | 2019-11-12 | 安徽广信农化股份有限公司 | A kind of hexazinone crystallization reactor |
-
2017
- 2017-06-29 CN CN201720772280.7U patent/CN207091325U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433758A (en) * | 2019-08-23 | 2019-11-12 | 安徽广信农化股份有限公司 | A kind of hexazinone crystallization reactor |
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