CN206778389U - A kind of process units of 3 ethylmercapto group butyraldehyde - Google Patents
A kind of process units of 3 ethylmercapto group butyraldehyde Download PDFInfo
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- CN206778389U CN206778389U CN201720597554.3U CN201720597554U CN206778389U CN 206778389 U CN206778389 U CN 206778389U CN 201720597554 U CN201720597554 U CN 201720597554U CN 206778389 U CN206778389 U CN 206778389U
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- storage tank
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- crotonaldehyde
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Abstract
The utility model discloses a kind of process units of 3 ethylmercapto group butyraldehyde, including coil reactor, condenser and the finished product storage tank being sequentially communicated；Also include ethyl mercaptan storage tank, crotonaldehyde storage tank, catalyst storage tank and corresponding ethyl mercaptan measuring pump, crotonaldehyde measuring pump and catalyst dosing pump；Ethyl mercaptan storage tank, crotonaldehyde storage tank and catalyst storage tank are communicated to the material inlet of coil reactor by ethyl mercaptan measuring pump, crotonaldehyde measuring pump and catalyst dosing pump respectively, the material outlet of coil reactor is communicated to the material inlet of condenser, and the material outlet of condenser is communicated to the material inlet of finished product storage tank.The utility model process units is simple, good leak tightness, security are more preferable, and floor space is few, and the product quality produced with this is high, stable yield.
Description
Technical field
The utility model belongs to technical field of chemical, and in particular to a kind of process units of 3- ethylmercapto groups butyraldehyde.
Background technology
3- ethylmercapto group butyraldehyde is the required intermediate of cyclohexenone analog herbicide clethodim and sethoxydim.Cyclohexenone analog removes
Careless agent has high selectivity, can prevent and treat a variety of grassy weeds, including annual gramineous weed and grassy weed for many years,
And to dicotyledonous crops safety, it is a kind of efficient, low toxicity, the herbicide of low-residual.
At present, the synthesis main technique of the 3- ethylmercapto group butyraldehyde is：
United States Patent (USP) US4440566 and Chinese document《The progress of synthesis of herbicide clethodim》Introduce, with crotonaldehyde
It is raw material reaction synthesis 3- ethylmercapto group butyraldehyde with ethyl mercaptan, ethyl mercaptan and crotonaldehyde are inside tank reactor, by stirring,
Under catalyst action, 30 degree reaction generation 3- ethylmercapto group butyraldehyde, then with dimethyl malenate cyclic condensation, then carry out alkaline hydrolysis and
Acidifying decarboxylation can obtain target product triketone (formula A).The process route production method falls behind, and working condition is poor, exothermic heat of reaction
Amount is big, it is necessary to dropwise reaction, wastes heat, production time length, intermittent reaction, due to need to use with it is strong, hold
The ethyl mercaptan of long stink does raw material, causes whole production process to be required for considering to handle ethyl mercaptan gas, adds tail
Gas disposal difficulty.
And in terms of production equipment, the operation that traditional tank reactor prepares 3- ethylmercapto group butyraldehyde is commonly used at present, due to making
It is traditional tank reactor, the problem of in order to more preferably remove reaction heat, it has to cooled down using coil pipe, and take drop
The method for adding ethyl mercaptan, prevent reaction from concentrating heat release.In addition to using tank reactor, it is necessary to be equipped with head tank, be added dropwise
The facilities such as tank, chuck therein need to be incubated, the operation such as cooling.Complete equipment space-consuming is big, and sealing is poor, production efficiency
It is low.
The content of the invention
Technical problem to be solved in the utility model is：A kind of process units of 3- ethylmercapto groups butyraldehyde, production dress are provided
Put the product quality height that simple, good leak tightness, security are more preferable, and floor space is few, are produced with this, stable yield.
In order to solve the above technical problems, the technical solution of the utility model is：
A kind of process units of 3- ethylmercapto groups butyraldehyde, including coil reactor, condenser and the finished product storage tank being sequentially communicated；
Also include ethyl mercaptan storage tank, crotonaldehyde storage tank, catalyst storage tank and corresponding ethyl mercaptan measuring pump, crotonaldehyde measuring pump and urge
Agent measuring pump；Ethyl mercaptan storage tank, crotonaldehyde storage tank and catalyst storage tank pass through ethyl mercaptan measuring pump, crotonaldehyde measuring pump respectively
The material inlet of coil reactor is communicated to catalyst dosing pump, the material outlet of coil reactor is communicated to the thing of condenser
Expect import, the material outlet of condenser is communicated to the material inlet of finished product storage tank.
Preferably, described coil reactor includes the main body of coil reactor, and body interior is chamber, and body top is opened
Provided with conduction oil outlet and material outlet, bottom offers heat conductive oil inlet and material inlet；Coil pipe is provided with main body inner wall,
Coil pipe both ends are respectively communicated with material inlet and material outlet；Some mixed cells and some guiding devices are additionally provided with coil pipe；
Counterbalance valve is provided with material outlet.Counterbalance valve can adjust the reaction pressure in coil reactor.
Coil reactor inwall is provided with the coil pipe of stainless steel seamless pipe manufacture, and material conveying and anti-is carried out inside coil pipe
Should, it is outside that reaction temperature is kept by conduction oil, every 20 meters of supporting 1 meter of mixed cells inside coil pipe, strengthen mass transfer, more added with
Carried out beneficial to reaction.A guiding device also is set every 5 meters inside coil pipe, is advantageous to import slow material is flowed at tube wall
The middle part of pipeline radial direction, improve fluid mixing velocity.
Preferably, described mixed cell is SK mixed cells, SV mixed cells or SL static mixers；Most elect SK as
Mixed cell.
Preferably, described guiding device is the hollow conical round table being built in coil pipe.
Preferably, described condenser is tubular heat exchanger.
By adopting the above-described technical solution, the beneficial effects of the utility model are：
1. the material reaction of the utility model design is carried out in closed pipeline, and keeps certain reaction pressure, keep away
The problem of having exempted from ethyl mercaptan vaporization, and is fed by measuring pump continuous metering, prevents second when the single batch of intermittent reaction feeds intake
The leakage problem of mercaptan, operating environment can be improved；
2. effectively solving heat transfer problem, reaction process is accelerated：Traditional tank reactor prepares 3- ethylmercapto group fourths
The operation of aldehyde is due to using traditional tank reactor, the problem of in order to more preferably remove reaction heat, it has to using coil pipe
Cooling, and the method that ethyl mercaptan is added dropwise is taken, prevent reaction from concentrating heat release；And process units is due to itself very big ratio surface
Product can fundamentally solve reactant heat transfer problem, and two kinds of components are proportionally fed, and reaction density is big, and reaction is instantaneous complete
Into；
3. raising reaction temperature can be realized, the speed of reaction is effectively improved：The mixed cell set inside coil pipe can be with
Strengthen mass transfer；One guiding device is set, is advantageous to, the middle part for flowing slow material import pipe radial direction at tube wall, improve stream
Body mixing velocity；Again because reaction coefficient is relevant with temperature with catalyst, temperature, which raises 10 degree of reaction speeds, can accelerate 2~4
Times, this process units is provided with counterbalance valve and can carry out pressurization and can be risen by conduction oil in process of production in equipment
Temperature insulation, therefore reaction speed can be improved.
4. reducing reaction unit volume, increase production security：Batch tank reactor is used in the prior art, daily
4 batch materials are produced, every batch materials charging time 2 hours, time for adding 2 hours, 4~5 hours reaction time, blowing 1 hour, always
10~12 hours when sharing, each equipment throws 2 batch materials, it is necessary to 2 consersion units, every equipment volume about 1.5 daily
Cube, material loads 1 cube, and material overall volume is 4 cubes, and 2 complete equipment total measurement (volume)s are about 3000 liters, and framework takes up an area face
Product is 50 square metres, high 3.5 meters；Head tank, dropping tank, chuck etc. are also needed to, and it also requires the operation such as insulation, cooling；And
4 cubes of material is equally produced using the coil reactor of this method daily, just 167 liters per hour, 3 liters of ability per minute, often
Just 0.05 liter of second.Reaction time is 10 minutes, and equipment volume only has 30 liters, and total floor space is 20 square metres, 4 meters of height.
Therefore, the utility model process units is simple, good leak tightness, security are more preferable, and floor space is few, is produced with this
Product quality is high, stable yield.
Brief description of the drawings
Fig. 1 is the structural representation of the utility model embodiment；
Fig. 2 is the structural representation of guiding device in the utility model；
Wherein, 1- ethyl mercaptans storage tank；2- crotonaldehyde storage tanks；3- catalyst storage tanks；4- ethyl mercaptan measuring pumps；5- crotonaldehyde meters
Measure pump；6- catalyst dosing pumps；7- coil reactors；8- heat conductive oil inlets；9- conduction oil outlets；10- coil pipes；11- materials enter
Mouthful；12- material outlets；13- condensers；14- finished product storage tanks；15- counterbalance valves；16- guiding devices.
Embodiment
With reference to the accompanying drawings and examples, the utility model is expanded on further.
As depicted in figs. 1 and 2, a kind of process units of 3- ethylmercapto groups butyraldehyde,
Including coil reactor 7, condenser 13 and the finished product storage tank 14 being sequentially communicated；Also include ethyl mercaptan storage tank 1, crotons
Aldehyde storage tank 2, catalyst storage tank 3 and corresponding ethyl mercaptan measuring pump 4, crotonaldehyde measuring pump 5 and catalyst dosing pump 6；Second sulphur
Alcohol storage tank 1, crotonaldehyde storage tank 2 and catalyst storage tank 3 pass through ethyl mercaptan measuring pump 4, crotonaldehyde measuring pump 5 and catalyst gauge respectively
Amount pump 6 is communicated to the material inlet of coil reactor 7, and the material that the material outlet of coil reactor 7 is communicated to condenser 13 enters
Mouthful, the material outlet of condenser 13 is communicated to the material inlet of finished product storage tank 14.
Including coil reactor 7, coil reactor 7 includes coil reactor main body, and body interior is chamber, body top
Conduction oil outlet 9 and material outlet 12 are offered, bottom offers heat conductive oil inlet 8 and material inlet 11；Set in main body inner wall
Coil pipe 10 is equipped with, the both ends of coil pipe 10 are respectively communicated with material inlet 11 and material outlet 12；If it is additionally provided with dry-mixing in coil pipe 10
Unit and some guiding devices 16；Counterbalance valve 15 is provided with material outlet 12.
In actual production, crotonaldehyde is passed through by crotonaldehyde measuring pump 5 with 87.5 kilograms per hour of flow, triethylamine
Catalyst dosing pump 6 is with 2.5 kilograms of flows per hour, and ethyl mercaptan is by ethyl mercaptan measuring pump 4 with 77.7 kilograms per hour of stream
Amount, well mixed into coil reactor 7, it is 80 DEG C to keep reaction temperature, is 10 points in the internal stops time of coil reactor 7
Clock, material control 20 kilograms of reaction pressure by the counterbalance valve 15 on material outlet 12, and reacting rear material is cold by condenser 13
Coagulate to entering finished product storage tank 14 after 30 DEG C.Finished product content reaches 98.5%, is directly used in and reacts in next step.
It should be understood that these embodiments are merely to illustrate the utility model rather than limitation the scope of the utility model.This
Outer to should be understood that after the content of the utility model instruction has been read, those skilled in the art can make each to the utility model
Kind change or modification, these equivalent form of values equally fall within the application appended claims limited range.
Claims (6)
- A kind of 1. process units of 3- ethylmercapto groups butyraldehyde, it is characterised in that：Including be sequentially communicated coil reactor, condenser and Finished product storage tank；Also include ethyl mercaptan storage tank, crotonaldehyde storage tank, catalyst storage tank and corresponding ethyl mercaptan measuring pump, crotonaldehyde Measuring pump and catalyst dosing pump；The ethyl mercaptan storage tank, crotonaldehyde storage tank and catalyst storage tank pass through the ethyl mercaptan respectively Measuring pump, crotonaldehyde measuring pump and catalyst dosing pump are communicated to the material inlet of the coil reactor, the coil pipe reaction The material outlet of device is communicated to the material inlet of the condenser, and the material outlet of the condenser is communicated to the finished product storage tank Material inlet.
- 2. the process units of 3- ethylmercapto groups butyraldehyde as claimed in claim 1, it is characterised in that：The coil reactor includes disk The main body of pipe reactor, the body interior are chamber, and the body top offers conduction oil outlet and material outlet, bottom Offer heat conductive oil inlet and material inlet；Coil pipe is provided with the inwall of the main body, the coil pipe both ends are respectively communicated with The material inlet and the material outlet；Some mixed cells and some guiding devices are additionally provided with the coil pipe；It is described Counterbalance valve is provided with material outlet.
- 3. the process units of 3- ethylmercapto groups butyraldehyde as claimed in claim 2, it is characterised in that：The mixed cell mixes for SK Unit, SV mixed cells or SL static mixers.
- 4. the process units of 3- ethylmercapto groups butyraldehyde as claimed in claim 3, it is characterised in that：The mixed cell mixes for SK Unit.
- 5. the process units of 3- ethylmercapto groups butyraldehyde as claimed in claim 2, it is characterised in that：The guiding device is to be built in Hollow conical round table in coil pipe.
- 6. the process units of 3- ethylmercapto groups butyraldehyde as claimed in claim 1, it is characterised in that：The condenser exchanges heat for tubulation Device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548335A (en) * | 2020-05-19 | 2020-08-18 | 广东省肇庆华格生物科技有限公司 | Methyl/ethyl maltol chlorination section production facility |
-
2017
- 2017-05-25 CN CN201720597554.3U patent/CN206778389U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548335A (en) * | 2020-05-19 | 2020-08-18 | 广东省肇庆华格生物科技有限公司 | Methyl/ethyl maltol chlorination section production facility |
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