CN206642724U - Continuous acylation synthesizes the device of pretilachlor - Google Patents
Continuous acylation synthesizes the device of pretilachlor Download PDFInfo
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- CN206642724U CN206642724U CN201720415918.1U CN201720415918U CN206642724U CN 206642724 U CN206642724 U CN 206642724U CN 201720415918 U CN201720415918 U CN 201720415918U CN 206642724 U CN206642724 U CN 206642724U
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Abstract
Pretilachlor preparation field is the utility model is related to, discloses a kind of device of continuous acylation synthesis pretilachlor, the device includes：Reactor, the feeding line connected with the reactor, the pipeloop (2) connected with the reactor and the discharging pipeline (3) connected with the reactor bottom；One end of the pipeloop (2) connects with the top of reactor, the other end connects with the bottom of reactor, heat exchanger (4) is connected with the pipeloop (2), the heat exchanger (4) is used for the circulation logistics that cooling flows through pipeloop (2).The device of continuous acylation synthesis pretilachlor provided by the utility model, not only operating automation degree is high, simple to operate, and floor space is small, saves manpower while ensureing that acylated product quality is stable, is very suitable for commercial Application.
Description
Technical field
Pretilachlor preparation field is the utility model is related to, in particular it relates to the device of continuous acylation synthesis pretilachlor.
Background technology
Pretilachlor is a kind of efficient, low toxicity, the special selective sprouting stage herbicide in rice field, belongs to conduction type herbicide.Third grass
The chemical name of amine：Chloro- 2 ', the 6 '-diethyl-N- of 2- (2- Amongs)-N- acetyl group aniline, external adopted name：
Pretiachlor, trade name have：Rifit solnet.Succeeded in developing by vapour Ba-Jia Ji companies of Switzerland in 1979, be conduct
Transplanting rice herbicide and the acetamide-group herbicides developed, available for the weeding of either manually or mechanically transplanting rice field, it can prevent and kill off big
Majority is mainly weeds in paddy field, such as sedge and a variety of broad leaved weeds, is used together with safener fenclorim, can improve this
Medicament can prevent and kill off rice terrace moleplant seed, special-shaped nutgrass flatsedge, Monochoria vaginalis and yak grass etc. to the security of rice bud paddy and seedling.
The synthetic route of pretilachlor initiation material used by, mainly there is chlorethanol route and ehter bond route.
A kind of pretilachlor new technique for synthesizing disclosed in CN102408352A, with 2,6- diethylanilines and ethylene glycol ether in copper vanadium
12~24h is reacted under catalyst action and obtains 2,6- diethylbenzene amido ethyl propyl ethers, then synthesizes pretilachlor.
The method of synthesizing herbicide pretilachlor by one-pot disclosed in CN102173998A, by 2,6- diethylanilines with highly basic non-
Reaction generation disodium iminodiacetic in proton solution, then reacts generation 2,6- diethylbenzene amido ethyl propyls with chloroethyl propyl ether
Ether, intermediate without isolation, occur acylation reaction with chloracetyl chloride again in same reactor, obtain pretilachlor.
The process route for the synthesis pretilachlor reported at present is mainly first synthetic intermediate 2,6- diethylbenzenes amido propyl group
Ether reacts with chloracetyl chloride again, and pretilachlor is made, and most of using batch process production.Although at present to acylation reaction route compared with
For maturation, but using needing to turn the auxiliary operations such as material and discharging, cycle length, human users' frequency during batch process production pretilachlor
Numerous and batch products quality is unstable, easily causes the loss of material and energy, is unfavorable for producing on a large scale.Therefore, need badly open
The simple efficient device for being used for pretilachlor industrialized production of hair.
Utility model content
The purpose of this utility model be overcome it is existing synthesis pretilachlor during, the cycle length, human users frequently and batch
A kind of the defects of unstable product quality, there is provided device of simple efficient continuous acylation synthesis pretilachlor.
The utility model provides a kind of device of continuous acylation synthesis pretilachlor, and the device includes：Reactor, with it is described anti-
Feeding line, the pipeloop connected with the reactor and the discharging connected with the reactor bottom for answering kettle to connect
Pipeline；One end of the pipeloop connects with the top of reactor, and the other end connects with the bottom of reactor, the circulation pipe
Heat exchanger is connected with line, the heat exchanger is used to cool down the circulation logistics for flowing through pipeloop.
Preferably, the reactor includes the reactor body with cavity structure, is arranged on reactor body interior
Agitating unit and the stirring motor for driving agitating unit, the agitating unit are used for material in stirred autoclave.
Preferably, the stirring motor is arranged at the top of reactor outer body.
Preferably, the agitating unit includes puddler and along the axially arranged agitator of puddler.
Preferably, the agitator includes that axially propeller agitator setting up and down and turbine type stir along puddler
Device.
Preferably, the reactor inner body wall is provided with baffle plate, and the quantity of the baffle plate is 2-4 blocks.
Preferably, the quantity of the feeding line is at least 2.
Preferably, the quantity of the feeding line is 4.
Preferably, be provided with first flowmeter and the first regulating valve on every feeding line, the first flowmeter and
First regulating valve is used for the flow for controlling reactor to feed.
Preferably, second flowmeter and the second regulating valve are provided with the discharging pipeline, the second flowmeter and the
Two regulating valves are used for the flow for controlling reactor to discharge.
Inventor of the present utility model has found in research process, in the technique of existing production pretilachlor, using interval
Method, because 2,6- diethylbenzene amido propyl ethers and chloracetyl chloride reaction synthesis pretilachlor are a kind of quick and strong exothermal reactions,
Temperature of reaction system can be caused constantly to raise if reaction heat can not remove in time during continuous production, runaway reaction, or even have super
The risk of warm slug.In addition, for the synthetic system of pretilachlor, using the preferable pusher stirring of the utility model and turbine type
The mode combined is stirred, is more beneficial for improving product purity and yield, thus it is speculated that its reason is probably due to this kind of preferable stirring
Mode can increase axial circulation lifting rate in reactor, improve the shear effect of stirring, prevent the generation of whirlpool, make in reaction
Oil phase and aqueous phase be sufficiently mixed, while the solid particle of generation is reached most uniform suspension.
The plant area of continuous acylation synthesis pretilachlor provided by the utility model is small, stable in the acylated product quality of guarantee
While save manpower, not only operating automation degree is high, simple to operate, and obtained pretilachlor product purity and yield compared with
Height, it is very suitable for commercial Application.
Other features and advantages of the utility model will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Accompanying drawing be for provide it is bright to utility model further understand, an and part for constitution instruction is and following
Embodiment be used to explain the utility model together, but do not form to limitation of the present utility model.In the accompanying drawings：
Fig. 1 is a kind of device of the continuous acylation synthesis pretilachlor of embodiment provided by the utility model.
Description of reference numerals
101- reactor body 2- pipeloops 3- discharging pipelines
4- heat exchanger 51- puddler 52- propeller agitators
53- turbine agitator 6- stirring motor 7- baffle plates
8- first flowmeters 9- the first regulating valve 10- second flowmeters
11- the second regulating valve 12- forced circulation pumps
Embodiment
Specific embodiment of the present utility model is described in detail below.It is it should be appreciated that described herein
Embodiment is merely to illustrate and explained the utility model, is not limited to the utility model.
The end points of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
In the utility model, in the case where not making opposite explanation, the noun of locality such as " upper and lower " used typically refers to join
Examine shown in the drawings upper and lower, the noun of locality used typically refers to top, the bottom shown in refer to the attached drawing such as " top, bottom ", makes
The noun of locality such as " inside and outside " refers to the inside and outside of the profile relative to each part in itself.
The utility model provides a kind of device of continuous acylation synthesis pretilachlor, and the device includes：Reactor, with it is described anti-
Feeding line, the pipeloop 2 connected with the reactor and the discharging connected with the reactor bottom for answering kettle to connect
Pipeline 3；One end of the pipeloop 2 connects with the top of reactor, and the other end connects with the bottom of reactor, the circulation
Heat exchanger 4 is connected with pipeline 2, the heat exchanger 4 is used to cool down the circulation logistics for flowing through pipeloop 2.
And what the synthesis pretilachlor of currently available technology used is intermittent reaction, intermittent reaction is by by 2,6- bis-
Ethylo benzene amido propyl ether (amidogen ether), alkali source and solvent are put into batch reactor, chloracetyl chloride are slowly added dropwise, due to this
Method is quick and strong exothermal reaction, if rate of addition is too fast to cause temperature rapid increase, can not obtain pretilachlor production
Product.Prior art typically reduces reaction temperature by setting inner coil pipe cooler in kettle.Set using batch production device
Standby utilization rate is relatively low, and batch operation is cumbersome, and production efficiency is too low.
Using device provided by the utility model, reaction raw materials are entered in reactor by feeding line to be reacted, instead
The product that should be obtained is divided into two tunnels, respectively circulates logistics a and product stream b, and circulation logistics a flows through pipeloop 2 and passed through
Cross heat exchanger 4 and cool down Posterior circle time reactor, to reduce reaction temperature in reactor；Product stream b completes liquid stream as acylated
Through discharging, pipeline 3 goes out device.
There is no particular limitation to the reactor for the utility model, can be various structures commonly used in the art
Reactor, it is preferable that the reactor includes the reactor body 101 with cavity structure, is arranged in reactor body 101
The agitating unit in portion and the stirring motor 6 for driving agitating unit, the agitating unit are used for material in stirred autoclave.
There is no particular limitation for set location of the utility model to the stirring motor 6, as long as stirring can be driven single
Member, preferably described stirring motor 6 are arranged on the outside top of reactor body 101, and the further preferred stirring motor 6 is set
Put in the middle position of the outside top of reactor body 101.It can not only be realized using the utility model preferred embodiment
The high efficiency drive of agitating unit, additionally it is possible to be not take up the internal volume of reactor body 101 completely.
According to device provided by the utility model, it is preferable that the inwall of reactor body 101 is provided with baffle plate 7.Stirring
During mixing, material can produce centrifugal force with the rotation of puddler, and formation puddler center material liquid surface is low, close to reactor
Material liquid surface is high at inwall, and therefore, the utility model preferably sets baffle plate 7 in the inwall of reactor body 101, and " whirlpool " is by significantly
Weaken, improve stirring efficiency to a certain extent.
The utility model is not required particularly the specific set location of the baffle plate, as long as close to reactor body
101 inwalls, the internal cavity volume of reactor body 101 will not be taken by being set close to the inwall of reactor body 101.
The utility model has no particular limits to the quantity of the baffle plate 7, can be 2-4 blocks, preferably 4 pieces, enter one
Step preferably 4 pieces of baffle plates 7 are uniformly arranged along the inwall ring of reactor body 101.
According to device provided by the utility model, the agitating unit can be including puddler 51 and along puddler 51 axially
The agitator of setting.
According to a kind of preferred embodiment of the present utility model, the agitator includes axially setting up and down along puddler 51
Propeller agitator 52 and turbine agitator 53.
For synthesizing pretilachlor system, using the preferable agitating unit of the utility model, upper strata is stirred to be pusher, lower floor
Stirred for turbine type, axial circulation lifting rate in reactor can be increased, improve the shear effect of stirring, prevent the production of whirlpool
It is raw, it is sufficiently mixed the oil phase (organic phase) in reaction and aqueous phase (inorganic phase), while the solid particle of generation is reached most equal
Even suspension, can cause obtained pretilachlor product purity and yield further improves.
The concrete structure of propeller agitator and turbine agitator described in the utility model is those skilled in the art
Known, the utility model will not be repeated here.
There is no particular limitation for quantity of the utility model to the feeding line, and those skilled in the art can be according to tool
The path that precursor reactant uses selects to react required material.It can select to be total to using same feeding line between different material
With charging, can also be fed respectively using different feeds pipeline.If two material contacts are reacted, the utility model is preferred
The two is fed respectively using different feeds pipeline.
According to a kind of preferred embodiment of the present utility model, the quantity of the feeding line is at least 2, preferably 4
Bar.
2,6- diethylbenzene amidos propyl ether, chloracetyl chloride, alkali source and solvent can be entered anti-by 2 feeding lines
Kettle is answered (to be fed jointly by a feeding line after chloracetyl chloride, alkali source and solvent mixing, 2,6- diethylbenzene amido propyl group
Ether is fed by a feeding line), can also be by 2,6- diethylbenzene amidos propyl ether, chloracetyl chloride, alkali source and solvent
In two kinds of mixing (be mutually mixed both do not chemically react) after fed jointly by a feeding line, it is remaining two kinds
Respectively enter reactor by 2 feeding lines, can also by 2,6- diethylbenzene amidos propyl ether, chloracetyl chloride, alkali source with
And solvent respectively enters reactor by 4 feeding lines.Preferably, 2,6- diethylbenzenes amido propyl ether, chloracetyl chloride, alkali
Source and solvent respectively enter reactor by 4 feeding lines.Using preferred embodiment of the present utility model, by 2,6- bis-
Ethylo benzene amido propyl ether, chloracetyl chloride, alkali source and solvent are fed respectively by 4 feeding lines, are more beneficial for generating pure
Degree and the higher pretilachlor of yield.
The regulating valve 9 of first flowmeter 8 and first, institute can be provided with according to the utility model, on every feeding line
State the flow that the regulating valve 9 of first flowmeter 8 and first is used to control reactor to feed.The He of first flowmeter 8 in the utility model
As long as the first regulating valve 9 can control the flow that reactor is fed, the utility model is no to its concrete structure particularly will
Ask.Those skilled in the art can select flowmeter and the concrete structure of regulating valve by concrete condition, will not be repeated here.
According to the utility model, the regulating valve 11 of second flowmeter 10 and second is provided with the discharging pipeline 3, described the
Two flowmeters 10 and the second regulating valve 11 are used for the flow for controlling reactor to discharge.
In the utility model, in order to realize the progress of continuous acylation reaction, preferably described first flowmeter 8 and first is adjusted
Save valve 9 and the regulating valve 11 of second flowmeter 10 and second control feed rate is equal with discharging flow.
According to device provided by the utility model, it is preferable that feed rate and discharging flow setting are chain.Control has been acylated
It is equal to the summation of feedstock amount into liquid produced quantity, ensures the balance of disengaging material in system.
Feed rate and discharging flow set it is chain carried out using this area conventional method, the utility model does not have to this
It is special to limit, for example, DCS electric signals can be utilized to interlock.
According to device provided by the utility model, it is preferable that pipeloop 2 and discharging pipeline 3 connect with reactor,
The discharging pipeline 3 is the bypass of the pipeloop 2, according to the acylation Synthesis liquid of the specifications control certain flow of product from going out
Expects pipe line 3 flows out, and the acylation Synthesis liquid of residual flow is recycled to reactor from pipeloop 2.
According to the utility model, can ensure to be acylated by setting forced circulation pump 12 on the main road of pipeloop 2
The output of Synthesis liquid.
The utility model can be by adjusting forced circulation pump 12 and by the regulating valve 11 of second flowmeter 10 and second
The flow that reactor discharges is controlled to cause 2,6- diethylbenzene amidos propyl ether, chloracetyl chloride, alkali source and total stream of solvent
The 5% of flow of the amount not higher than circulation logistics a, it is preferable that 2,6- diethylbenzene amido propyl ethers, chloracetyl chloride, alkali source and
The total flow of solvent is the 0.1-1% of circulation logistics a flow.Using this kind of preferred embodiment, the larger side of internal circulating load one
Face can guarantee that the purity of product, on the other hand can accelerate mass transfer, strengthen heat-transfer effect, be advantageous to react.
According to device provided by the utility model, there is no particular limitation to the heat exchanger 4 for the utility model, as long as energy
Enough coolings flow through the circulation logistics of pipeloop 2.By setting heat exchanger 4 on pipeloop 2, lead to cooling medium, energy
It is enough to remove acylation reaction liberated heat in time.
According to a kind of preferred embodiment of the present utility model, the heat exchanger 4 is tubular heat exchanger, acylated to complete liquid
Managed from heat exchanger 4 interior by managing outer logical chilled brine as heat transferring medium, reducing the temperature for being acylated and completing liquid.
According to the utility model, can by adjust heat exchanger 4 by 2,6- diethylbenzene amidos propyl ether, chloracetyl chloride,
Alkali source and the control of solvent reaction condition are in the range of -5 to 10 DEG C (preferably 0-5 DEG C), for example, be able to will be followed by heat exchanger 4
Ring logistics a heat exchange is cooled to 0-5 DEG C of Posterior circle to reactor.
Circulate logistics a flow and can be with the catalytic temperature of co- controlling, this reality by the temperature for circulating logistics a coolings
Being to provide one kind with new can control one kind in the range of -5 to 10 DEG C (preferably 0-5 DEG C) to be embodied reaction condition
Mode, the utility model are not limited to this.
Those skilled in the art can determine charging total flow according to actual production demand, determine to react with reference to the residence time
Kettle accumulates size, is required to select appropriate circular flow according to product specification.If for example, require that product purity is not less than
95%, then the total flow of 2,6- diethylbenzenes amido propyl ether, chloracetyl chloride, alkali source and solvent is circulation logistics a flow
Less than 5%.If reactor volume is 5000L, 2, the 6- diethylbenzenes amido propyl ether, chloracetyl chloride, alkali source with
And the total flow of solvent can be 1500-3500L/h, preferably 1750-3000L/h.
A kind of embodiment of the present utility model presented below, as shown in figure 1, raw material 2,6- diethylbenzenes amido third
Base ether (amidogen ether), chloracetyl chloride, liquid caustic soda and toluene are measured by first flowmeter 8 and the first regulating valve 9 is adjusted respectively with 600L/
H, 200L/h, 265L/h, 690L/h flow by 4 feeding lines are pumped to reactor body 101 respectively, and (volume is
In 5000L), the residence time is：2.3h.Reactor body 101 is internally provided with agitating unit, and the outside of reactor body 101 is pushed up
Portion middle position is provided with the stirring motor 6 for driving agitating unit, and agitating unit includes puddler 51 and along puddler 51
Axially propeller agitator 52 and turbine agitator 53 setting up and down, are uniformly arranged along the inwall ring of reactor body 101
There are 4 pieces of baffle plates 7.Raw material 2,6- diethylbenzene amidos propyl ether, chloracetyl chloride, liquid caustic soda and toluene lead in reactor body 101
Cross propeller agitator 52 and turbine agitator 53 to be stirred together for acting on, reaction resulting material is divided into two-way that (main road circulates
Bypass discharging pipeline 3 is set on pipeline 2, forced circulation pump 12, the flow of forced circulation pump 12 are set on the main road of pipeloop 2
For 800m3/ h, lift 15m), it is recycled to all the way as circulation logistics a by pipeloop 2 in reactor, circulation logistics a exists
It is recycled back to before reactor, passes through (the heat exchanger area 50m of tubular heat exchanger 42) heat exchange cooling, logistics a is circulated from heat exchange
Device 4 manage in by managing outer logical chilled brine and being used as heat transferring medium, circulation logistics a is cooled into 5 DEG C of Posterior circles to reactor (instead
It is 0-5 DEG C to answer kettle interior reaction temperature；Another way is controlled by the regulating valve 11 of second flowmeter 10 and second as product stream b,
Device is gone out by the pipeline 3 that discharges with 1760L/h flow.Analysis test is carried out to product stream b, the purity of obtained pretilachlor
It is higher with yield.
A kind of a kind of embodiment of prior art batch production pretilachlor presented below, under room temperature (25 DEG C),
Pretilachlor is produced using batch tank, by the ingredient proportion of embodiment 1, in 3000L reactor, every batch is separately added into amidogen ether
630L, liquid caustic soda 315L, toluene 890L, 200L chloracetyl chlorides are slowly added dropwise, it is cold that time for adding control is provided with inner coil pipe in 4h, kettle
But device, reaction temperature are controlled at -5~5 DEG C, and reaction obtains pretilachlor purity and yield is slightly below the utility model.In addition, using
Batch production device, utilization rate of equipment and installations is relatively low, and batch operation is cumbersome.
The device of continuous acylation synthesis pretilachlor provided by the utility model is can be seen that by above-mentioned comparison, is not only grasped
Make that automaticity is high, simple to operate, and obtained pretilachlor product purity and yield are higher.
Preferred embodiment of the present utility model, still, the utility model and unlimited is described in detail above in association with accompanying drawing
Detail in above-mentioned embodiment, can be to skill of the present utility model in range of the technology design of the present utility model
Art scheme carries out a variety of simple variants, and these simple variants belong to the scope of protection of the utility model.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, it can be combined by any suitable means.
In addition, it can also be combined between a variety of embodiments of the present utility model, as long as it is not disobeyed
Thought of the present utility model is carried on the back, it should equally be considered as content disclosed in the utility model.
Claims (10)
1. a kind of device of continuous acylation synthesis pretilachlor, it is characterised in that the device includes：
Reactor, the feeding line connected with the reactor, the pipeloop (2) connected with the reactor and with it is described
The discharging pipeline (3) of reactor bottom connection；
One end of the pipeloop (2) connects with the top of reactor, and the other end connects with the bottom of reactor, the circulation
Heat exchanger (4) is connected with pipeline (2), the heat exchanger (4) is used for the circulation logistics that cooling flows through pipeloop (2).
2. device according to claim 1, it is characterised in that the reactor includes the reactor sheet with cavity structure
Body (101), the internal agitating unit of reactor body (101) and the stirring motor (6) for driving agitating unit are arranged on,
The agitating unit is used for material in stirred autoclave.
3. device according to claim 2, it is characterised in that the stirring motor (6) is arranged on reactor body (101)
Outside top.
4. device according to claim 2, it is characterised in that the agitating unit includes puddler (51) and along puddler
(51) axially arranged agitator.
5. device according to claim 4, it is characterised in that the agitator includes dividing into along puddler (51) axial direction
The propeller agitator (52) and turbine agitator (53) put.
6. device according to claim 2, it is characterised in that reactor body (101) inwall is provided with baffle plate
(7), the quantity of the baffle plate (7) is 2-4 blocks.
7. according to the device described in any one in claim 1-6, it is characterised in that the quantity of the feeding line is at least
2.
8. device according to claim 7, it is characterised in that the quantity of the feeding line is 4.
9. device according to claim 7, it is characterised in that first flowmeter (8) is provided with every feeding line
With the first regulating valve (9), the first flowmeter (8) and the first regulating valve (9) are for controlling the flow that reactor is fed.
10. according to the device described in any one in claim 1-6, it is characterised in that be provided with the discharging pipeline (3)
Second flowmeter (10) and the second regulating valve (11), the second flowmeter (10) and the second regulating valve (11), which are used to control, reacts
The flow of kettle discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720415918.1U CN206642724U (en) | 2017-04-19 | 2017-04-19 | Continuous acylation synthesizes the device of pretilachlor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720415918.1U CN206642724U (en) | 2017-04-19 | 2017-04-19 | Continuous acylation synthesizes the device of pretilachlor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054296A (en) * | 2019-12-02 | 2020-04-24 | 河南金鹏化工有限公司 | Continuous production device and process for thiodicarb salinization reaction |
| CN114950320A (en) * | 2022-05-31 | 2022-08-30 | 浙江巨化技术中心有限公司 | Device and method for continuously synthesizing tetrafluoroethane-beta-sultone |
-
2017
- 2017-04-19 CN CN201720415918.1U patent/CN206642724U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054296A (en) * | 2019-12-02 | 2020-04-24 | 河南金鹏化工有限公司 | Continuous production device and process for thiodicarb salinization reaction |
| CN114950320A (en) * | 2022-05-31 | 2022-08-30 | 浙江巨化技术中心有限公司 | Device and method for continuously synthesizing tetrafluoroethane-beta-sultone |
| CN114950320B (en) * | 2022-05-31 | 2023-09-15 | 浙江巨化技术中心有限公司 | Device and method for continuously synthesizing tetrafluoroethane-beta-sultone |
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