CN107537423A - Continuous still reaction device and n-BuLi participate in the continuous still reaction system of production - Google Patents
Continuous still reaction device and n-BuLi participate in the continuous still reaction system of production Download PDFInfo
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- CN107537423A CN107537423A CN201710675542.2A CN201710675542A CN107537423A CN 107537423 A CN107537423 A CN 107537423A CN 201710675542 A CN201710675542 A CN 201710675542A CN 107537423 A CN107537423 A CN 107537423A
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Abstract
The invention provides the continuous still reaction system that a kind of continuous still reaction device and n-BuLi participate in production.Continuous still reaction device includes N number of successive reaction kettle for being sequentially connected in series setting, and each successive reaction kettle includes body, and body has reaction chamber, charging aperture, overfall and discharging opening；Wherein, N is >=2 natural number, and the overfall of 1 successive reaction kettle of N is connected with the charging aperture of n-th successive reaction kettle.This continuous still reaction device is applied to the chemical reaction that the active chemical substance of the properties such as n-BuLi participates in, it can need to select suitable number of successive reaction kettle to carry out continuous reaction according to reacting dose in actual production, not only reduce disposable transfer in the production of one-pot batch or a large amount of reaction raw materials are added dropwise for a long time, operation risk is reduced, improves security and reaction efficiency.
Description
Technical field
The present invention relates to organic synthesis field, joins in particular to a kind of continuous still reaction device and n-BuLi
With the continuous still reaction system of production.
Background technology
N-BuLi can be used for lithium-halogen and exchange as a highly basic as the lithiation reagent of the substrate containing active hydrogen
Reaction or lithium-metal transfer metallization reaction, are widely used in Synthetic Organic Chemistry and pharmaceuticals industry.In addition, n-BuLi
Polymerization catalyst, alkylating agent are also used as, triggers conjugated diene to carry out anionic polymerisation, for preparing low-cis-polybutadiene
Rubber, isoprene rubber, thermoplastic elastomer, thermosetting resin and coating etc..Generally speaking, n-BuLi is a kind of important
Chemical reagent, it is widely used in organic synthesis industry and Polymeric Industry.
However, the property of n-BuLi is very active, run into easily on fire when air or moisture.Operation to n-BuLi
It should carry out under the protection of the nitrogen or argon gas of isolation air and moisture, especially when high-volume uses n-BuLi, need to ensure anti-
Answer the strict anhydrous and oxygen-free of system, reduction personnel directly contact, definitely prevent material from leakage from triggering danger as far as possible.It is industrial at present big
Batch is produced using batch one-pot mostly using n-BuLi, generally requires disposable transfer or a large amount of normal-butyls are added dropwise for a long time
Lithium, process risk are higher.Specifically have as a drawback that：
1) one-pot reaction of batch, substantial amounts of n-BuLi are added dropwise in reactor, and material adds up more, exothermic heat of reaction amount
Greatly, it is dangerous high.
2) batch reactor volume is big, once material from leakage, potential safety hazard is big, and personnel withdraw difficulty.
3) batch reactor one-pot volume is big, and mixed effect is poor, and lithiation stability is poor, and yield is low, purity difference.
4) existing batch reaction, once middle tracking result is bad, whole kettle material all can be impacted.
5) lithiation temperature control is relatively low, and exothermic heat of reaction amount is big, and existing batch reactor heat exchange specific surface area is small, ultralow temperature control
System is difficult.
6) existing lithiumation production, automaticity is low, and rate of addition control stability is poor, labor intensive material resources and time.
7) batch reactor floor space is big, low space utilization, and equipment investment is high.
The content of the invention
It is a primary object of the present invention to provide a kind of continuous still reaction device and n-BuLi to participate in the continuous of production
Still reaction system, to solve the problems, such as the reaction safety difference of n-BuLi participation in the prior art.
To achieve these goals, according to an aspect of the invention, there is provided a kind of continuous still reaction device, the company
Continuous still reaction device includes：N number of successive reaction kettle for being sequentially connected in series setting, each successive reaction kettle include body, body tool
There are reaction chamber, charging aperture, overfall and discharging opening；Wherein, N be >=2 natural number, the overflow of the N-1 successive reaction kettle
Mouth is connected with the charging aperture of n-th successive reaction kettle.
Further, the charging aperture of the overfall of the N-1 successive reaction kettle and n-th successive reaction kettle passes through overflow pipe
Road is connected.
Further, it is sequentially connected in overfall and charging aperture on logical direction, the overfall of the N-1 successive reaction kettle
Higher than the charging aperture of n-th successive reaction kettle.
Further, multiple successive reaction kettles are horizontally disposed with, and are provided with protective gas on first successive reaction kettle and are entered
Vacuum extractor is provided with mouth or n-th successive reaction kettle.
Further, successive reaction kettle also includes agitating device, and agitating device includes puddler and agitating paddle, agitating paddle position
In reaction chamber, one end of puddler is connected with agitating paddle, and the other end extends to this in vitro and is connected with motor.
Further, successive reaction kettle also includes reacting kettle jacketing, and reacting kettle jacketing is set around the outer wall of body.
Further, reacting kettle jacketing corresponding to two neighboring successive reaction kettle is connected.
Further, successive reaction kettle also includes cooling coil, and cooling coil is arranged in reaction chamber, and around body
Inwall is set.
Further, cooling coil corresponding to two neighboring successive reaction kettle is connected.
Further, successive reaction kettle also includes monitoring element and holds the sleeve pipe of monitoring element, and sleeve pipe passes through body
Stretch into reaction chamber.
Further, monitoring element is electroheat pair, thermal resistance and/or thermometer.
Further, successive reaction kettle also includes pressure transmitter, and body also includes the pressure through hole being arranged on roof,
Pressure transmitter is connected and is arranged on the outer wall of body with pressure through hole.
To achieve these goals, according to an aspect of the invention, there is provided a kind of n-BuLi participates in the company of production
Continuous still reaction system, continuous still reaction system include continuous still reaction device, and continuous still reaction device is above-mentioned
A kind of continuous still reaction device；And feeding device, feeding device are connected with continuous still reaction device.
Further, continuous still reaction system also includes control device, and control device is connected with feeding device to control
The feed quantity of feeding device.
Further, control device is also connected with continuous still reaction device, to monitor the fortune of continuous still reaction device
Row state, and in continuous still reaction plant running exception stop feeding device feed.
Further, feeding device includes feedstock storage unit；Metering device, feedstock storage unit are placed on metering device
On, metering device is connected with control device so that metric results are fed back into control device；And feed pump, feedstock storage unit lead to
Cross feed pump with continuous still reaction device to be connected, feed pump is connected with control device to control feed pump by control device
Inlet amount.
Further, feedstock storage unit includes nitrogen blow valve port, and continuous still reaction system also includes product and collects dress
Put, product collecting device is arranged on the downstream of continuous still reaction device；Nitrogen blow valve port is connected with control device, for working as to enter
After material terminates, nitrogen blow valve port is opened by control device reaction product is blown in product collecting device.
Apply the technical scheme of the present invention, by the way that N number of successive reaction kettle is sequentially connected in series into setting, and cause N- continuously
The overfall of reactor is connected with the charging aperture of n-th successive reaction kettle so that material passes through first successive reaction kettle
Charging aperture enters first order reactor, and when volume reaches its overfall position, material passes through in overflow to next stage reactor
Reacted, reacted material is flowed out by discharging opening.This continuous still reaction device is applied to the properties such as n-BuLi and lived
The chemical reaction that bold and vigorous chemical substance participates in, it can be selected suitable number of according to the needs of real reaction amount in actual production
Successive reaction kettle carries out continuous reaction, not only reduces disposable transfer in the production of one-pot batch or is added dropwise for a long time a large amount of anti-
Raw material is answered, reduces operational risk, and improve reaction efficiency.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the structural representation of the continuous still reaction device in a kind of preferred embodiment of the present invention；With
And
Fig. 2 shows that n-BuLi participates in the continuous still reaction system reacted in another preferred embodiment of the invention
The structural representation of system；
Fig. 3 shows the detailed construction schematic diagram of each flow reactor in Fig. 1.
Wherein, above-mentioned accompanying drawing marks including the following drawings：
10th, successive reaction kettle；11st, body；111st, reaction chamber；112nd, charging aperture；113rd, overfall；114th, discharging opening；12、
Agitating device；13rd, reacting kettle jacketing；14th, cooling coil；15th, sleeve pipe；16th, pressure transmitter；
01st, continuous still reaction device；02nd, feeding device；03rd, control device；04th, product collecting device；
021st, feedstock storage unit；022nd, metering device；023rd, feed pump；020th, nitrogen blow valve port.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.The present invention is described in detail below in conjunction with embodiment.
As background technology is previously mentioned, the reaction that existing n-BuLi participates in is produced using batch one-pot more, is often needed
Disposably to shift or a large amount of n-BuLis are added dropwise for a long time, process risk is higher.In order to reduce the danger of this similar reaction
Property, in a kind of typical embodiment of the application, there is provided a kind of continuous still reaction device 01, as shown in figures 1 and 3,
The continuous still reaction device 01 includes N number of successive reaction kettle 10 for being sequentially connected in series setting, and each successive reaction kettle 10 includes this
Body 11, body 11 have reaction chamber 111, charging aperture 112, overfall 113 and discharging opening 114；Wherein, N is >=2 nature
Number, the overfall 113 of the N-1 successive reaction kettle 10 are connected with the charging aperture 112 of n-th successive reaction kettle 10.
Continuous still reaction device 01 provided herein, by the way that N number of successive reaction kettle 10 is sequentially connected in series into setting, and
So that the overfall 113 of the N-1 successive reaction kettle 10 is connected with the charging aperture 112 of n-th successive reaction kettle 10 so that thing
Material enters first order reactor by the charging aperture 112 of first successive reaction kettle 10, when volume reaches its position of overfall 113
When, by being reacted in overflow to next stage reactor, reacted material is flowed out material by discharging opening 114.It is this continuous
Still reaction device 01 is applied to the chemical reaction that the active chemical substance of the property such as n-BuLi participates in, can be with actual production
According to the needs of real reaction amount, select suitable number of successive reaction kettle 10 to carry out continuous reaction, not only reduce one-pot
A large amount of reaction raw materials are added dropwise in disposable transfer or long-time in batch production, reduce operational risk, and improve reaction effect
Rate.
In above-mentioned continuous still reaction device 01, the number N of successive reaction kettle 10 can be carried out according to actual condition sequence
Reasonable selection, can be 3,4,5 or 6, it is even more.The number of successive reaction kettle 10 of series connection is more, normal-butyl
The treating capacity of lithium is bigger.The overflow volume of each successive reaction kettle 10 can also rationally be set according to treating capacity, preferably
The overflow volume of each successive reaction kettle 10 is no more than 14L, and in the range of the overflow volume, material storage is few, if just in case occurring
Material from leakage, disposable, hazards are small.
Above-mentioned N number of successive reaction kettle 10 being serially connected, pass through respective overfall 113 and the successive reaction that is connected thereafter
The charging aperture 112 of kettle 10 is connected, it is achieved thereby that the continuous reaction of high-volume material.Specific overfall 113 and charging
The connection form of mouth 112 is unlimited, and any mode that can realize connection is applied to the application.It is a kind of preferable real in the application
Apply in example, the overfall 113 of the N-1 successive reaction kettle 10 passes through overflow pipe with the charging aperture 112 of n-th successive reaction kettle 10
Road is connected.The presence of overflow passage is easy to flexibly set the position of different successive reaction kettles 10.
In actual production, the concrete arrangement of N number of successive reaction kettle 10 being serially connected can be according to site area
The coordinated production of size or equipment room is rationally set.In a kind of preferred embodiment of the application, in overfall 113 with entering
Material mouth 112 is sequentially connected on logical direction, and the overfall 113 of the N-1 successive reaction kettle 10 is higher than n-th successive reaction kettle 10
Charging aperture 112.This preferred arrangement is flowed to next continuous anti-by Action of Gravity Field by previous successive reaction kettle 10
Kettle 10 is answered, saves energy consumption.
In the application another kind preferred embodiment, multiple successive reaction kettles 10 are horizontally disposed, and first continuous anti-
Answer to be provided with kettle 10 on gas atmosphere inlet or n-th successive reaction kettle 10 and be provided with vacuum extractor.When multiple continuous
When reactor 10 is horizontally disposed with, on first successive reaction kettle 10 being provided with gas atmosphere inlet can be easy to by the gas
Entrance applies positive pressure to multiple successive reaction kettles 10, so as to promote material to be circulated between multiple successive reaction kettles 10.And
Vacuum extractor is provided with n-th successive reaction kettle 10, negative pressure is taken out to multiple successive reaction kettles 10 above, equally can
Realize the continuous flow of material.
Above-mentioned successive reaction kettle 10 is in addition to charging aperture 112, reaction chamber 111, overfall 113 and discharging opening 114, root
There can also be multiple other different reaction accessories according to differential responses.Such as agitating device 12, specific agitating device 12
Design form can also optimize design according to being actually needed.In a kind of preferred embodiment of the application, such as Fig. 1 and figure
Shown in 3, successive reaction kettle 10 also includes agitating device 12, and agitating device 12 includes puddler and agitating paddle, and agitating paddle is positioned at anti-
Answer in chamber 111, one end of puddler is connected with agitating paddle, and the other end is extended to outside body 11 and is connected with motor.Stirring
The setting of device 12 is beneficial to be sufficiently mixed material, stirs, and so as to shorten the reaction time, improves reaction efficiency.Often
The rotating speed of agitating device 12 can adjust in platform successive reaction kettle 10, with suitable for different mixing demands.Specific body, agitating paddle
Specific number is unlimited, can be 2,3,4,6 etc., spirally can set or be symmetrical arranged.
Above-mentioned successive reaction kettle 10 is according to different reactions, it is necessary to meet different reaction temperature conditions, its temperature control mode
Using existing temperature control mode.In a kind of preferred embodiment of the application, successive reaction kettle 10 also includes reactor and pressed from both sides
Set 13, reacting kettle jacketing 13 are set around the outer wall of each successive reaction kettle 10.In a kind of preferred embodiment of the application, phase
Reacting kettle jacketing 13 corresponding to adjacent two successive reaction kettles 10 is connected.It is continuous anti-in a kind of preferred embodiment of the application
Kettle 10 is answered also to include cooling coil 14, cooling coil 14 is arranged in reaction chamber 111, and is set around the inwall of successive reaction kettle 10
Put.In a kind of preferred embodiment of the application, cooling coil 14 corresponding to two neighboring successive reaction kettle 10 is connected.
Above-mentioned a variety of temperature control modes be able to can also coordinate applicable with single use, and the application is preferably used cooperatively.The whole series dress
The temperature control method put is carried out by the way of internal cooling coil pipe 14 and the co- controlling of external reaction kettle chuck 13.For inner disk
Management and control temperature, cooling coil 14 corresponding to two neighboring successive reaction kettle 10 are connected, successive reaction that can be by refrigerant by N levels
The coil media import of kettle 10 enters the successive reaction kettle 10 of N levels, then connects step by step, finally by the successive reaction of the first order
The coil media outlet bleeder of kettle 10.For the temperature control of external reaction kettle chuck 13, the two neighboring correspondence of successive reaction kettle 10
Reacting kettle jacketing 13 be connected, refrigerant can be entered N cascades by the chuck medium entrance of the successive reaction kettle 10 of N levels
Continuous reactor 10, then connects step by step, finally by the first order successive reaction kettle 10 chuck media outlet bleeder.Respectively connect
Series sequence between continuous reactor 10 can carry out reasonable combination according to the process requirements of reality.
Above-mentioned continuous still reaction device 01 carries out continuous reaction by N number of successive reaction kettle 10 being arranged in series,
Through the security for improving reaction.In order to further improve the security of reaction, reaction risk is reduced, it is a kind of preferably in the application
Embodiment in, successive reaction kettle 10 also includes monitoring element and holds the sleeve pipe 15 of monitoring element, and sleeve pipe 15 passes through body
11 stretch into reaction chamber 111.The technological parameter that specific detecting element monitors according to needed for actual process situation is rationally set
Put.In a kind of preferred embodiment of the application, monitoring element is electroheat pair, thermal resistance and/or thermometer.Electroheat pair, thermoelectricity
Resistance and/or thermometer can reflect the operation conditions of continuous still reaction device 01 from the different aspect such as heat and temperature, if
The technique allowed band that actual temperature exceedes, so as to provide Risk-warning for the operation conditions of package unit.
In a kind of preferred embodiment, as shown in figure 3, above-mentioned successive reaction kettle also includes pressure transmitter 16, body
Also include the pressure through hole being arranged on roof, pressure transmitter 16 is connected and is arranged on the outer wall of body with pressure through hole.
Pressure transmitter be it is a kind of convert pressure into pneumatic signal or electromotive signal is controlled equipment with teletransmission, can be by pressure measurement member
The physical pressure parameters such as gas that part sensor is experienced, liquid are transformed into the electric signal of standard, to supply indicator alarm, note
Record instrument, the secondary meter such as adjusting apparatus measure, indicates and procedure regulation.By the outer wall that pressure transmitter is arranged on to body
On, and the gas pressure inside successive reaction kettle is perceived by pressure through hole on body roof, and then being capable of the company of monitoring in real time
Reaction pressure inside continuous reactor, the normal operation for W-response device provide Risk-warning.Specifically, pressure transmitter
It can be connected through a screw thread and be fixed on flow reactor with pressure through hole.
Electroheat pair, electrothermal resistance and/or thermometer in above-mentioned monitoring element sleeve pipe can bases with above-mentioned pressure transmitter
Needs of production, while be arranged on each successive reaction kettle, carried out in real time in order to the operation conditions of each successive reaction kettle
Monitoring.
In the application, the material of each successive reaction kettle 10 can be stainless steel or Hastelloy.In special process requirement
, can be with inner liner polytetrafluoroethylene, with the reaction suitable for all kinds of corrosivity or the participation of acid material under operating mode.
In another typical embodiment of the application, there is provided the continuous autoclave that a kind of n-BuLi participates in production is anti-
System is answered, as shown in Fig. 2 the continuous still reaction system includes：Continuous still reaction device and feeding device 02, wherein connecting
Continuous still reaction device is the continuous still reaction device of any of the above-described kind of the application, feeding device 02 and continuous still reaction device
It is connected.The above-mentioned continuous still reaction device of the application is connected with feeding device 02, can realize that n-BuLi is this
Serialization, the reaction of batch of the active material of chemical property, and it is safe.
On the basis of above-mentioned security is improved, in order to ensure that the safety of a whole set of reaction system to a greater extent
Property, in a kind of preferred embodiment of the application, continuous still reaction system also includes control device 03, the control device 03 with
Feeding device 02 is connected to control the feed quantity of feeding device 02.The inlet amount of butyl lithium is set in control device 03,
Feeding device 02 is fed according to the instruction of control device 03, and charging stability is good, and the degree of accuracy is high.Material is led to by material device
Cross supply lines and be delivered in continuous still reaction device and reacted.Specific control device 03 can be PLC control cabinet.
In a kind of preferred embodiment of the application, as shown in Fig. 2 above-mentioned control device 03 also fills with continuous still reaction
Put connected, to monitor the running status of continuous still reaction device, and stop supplying in continuous still reaction plant running exception
Expect the feed of device 02.The process status of continuous still reaction device is such as pressed by the monitoring element on each successive reaction kettle 10
Power transmitter and thermal resistance are monitored, if the technique allowed band that actual temperature or pressure exceed, control device 03 can the
One time noted abnormalities, and voluntarily stops being fed and alarming, ensure that the security of package unit to the full extent, and this is big to being related to
The reaction of batch n-BuLi production is particularly important.
The specific setting form of above-mentioned feeding device 02 is depending on actual condition.In a kind of preferred embodiment of the application
In, as shown in Fig. 2 feeding device 02 includes feedstock storage unit 021, metering device 022 and feed pump 023, raw material storage dress
Set to 0 21 to be placed on metering device 022, metering device 022 is connected with control device 03 so that metric results are fed back into control dress
Set to 03；Feedstock storage unit 021 is connected by feed pump 023 with continuous still reaction device, feed pump 023 and control device 03
It is connected to control the inlet amount of feed pump 023 by control device 03.
In above preferred embodiment, metering device 022 can be specifically weigher, preferably electronic scale.Specific charging
Weight is set in control device 03, and feed pump 023 carries out dnockout according to the instruction of control device 03, by metering device
The data feedback of 022 (electronic scale) forms closed-loop control, charging stability is good, and the degree of accuracy is high to control device 03.
Because all operations of n-BuLi are required for carrying out under the isolation protection such as air and the nitrogen of moisture or argon gas.
Thus, the continuous still reaction system that above-mentioned n-BuLi participates in reaction is carried out under the atmosphere of protective gas.
In a kind of preferred embodiment of the application, feedstock storage unit 021 includes nitrogen blow valve port 020, above-mentioned continuous still reaction system
System also includes product collecting device 04, and the product collecting device 04 is arranged on the downstream of continuous still reaction device；Nitrogen purges
Mouth 020 is connected with control device 03, for after charging terminates, opening nitrogen blow valve port 020 by control device 03 will reaction
Product is blown in product collecting device 04.After charging terminates, PLC equal controllers 03 can voluntarily switch, and open nitrogen blow valve port
020 is blown to system material in product reception device, avoids n-BuLi from being caused danger with air contact.
In a kind of preferred embodiment of the application, the continuous still reaction device of the application includes 4 grades of overflow reactors,
Specifically include including：Charging aperture, overflow passage, reactor cavity, reacting kettle jacketing, agitating paddle, cooling coil, discharging opening, stir
Mix motor and thermometer boss.Material enters first order reactor by charging aperture, when volume reaches overfall position, thing
Material is flow in next stage reactor by overflow passage to be reacted, and reacted material is flowed out by products export；Package unit
Temperature control method carried out by the way of internal cooling coil pipe and external reaction kettle chuck co- controlling, for inner disk management and control
Temperature, refrigerant enter fourth stage overflow kettle by coil media import, connect step by step, finally export bleeder by coil media；It is right
In external reaction kettle chuck temperature control, refrigerant enters fourth stage overflow kettle by chuck medium entrance, connects, be finally situated between by chuck step by step
Matter exports bleeder；Each kettle series sequence can carry out selection combination according to the process requirements of reality.The mixing of material passes through every
The stirring of platform kettle is controlled, and every kettle speed of agitator is adjustable to be applied to different mixing demands.Temperature in every reactor
Degree is measured by thermometer boss.Reactor material is the material such as stainless steel, Hastelloy, the work of special process requirement
Condition, can be with inner liner polytetrafluoroethylene, suitable for all kinds of corrosivity, the reaction of acid material participation.
In another preferred embodiment, there is provided a kind of continuous still reaction system.The system includes：It is sequentially connected
PLC control cabinet, electronic scale, Raw material pail, feed pump, continuous tank reactor and product receiving tank.The inlet amount of butyl lithium
Set in PLC control system, feed pump carries out dnockout according to the instruction of switch board, and specific feed weight is by electronic scale
Data feedback to PLC control system, form closed-loop control, charging stability is good, and the degree of accuracy is high；Material is defeated by pipeline by pump
Deliver in continuous tank reactor and reacted, process status can be supervised by the pressure transmitter on reactor and thermal resistance
Survey, if the technique allowed band that actual temperature or pressure exceed, PLC control system can note abnormalities the very first time, voluntarily stop
Pump is simultaneously alarmed, and ensure that the security of package unit to the full extent, more particularly to the reaction of high-volume n-BuLi production
It is particularly important.After charging terminates, PLC control system can voluntarily switch, and system material is blown to product and connect by opening nitrogen blow valve port
In closed cans, n-BuLi is avoided to be caused danger with air contact.
Above-mentioned continuous still reaction system produces suitable for high-volume n-BuLi, and charging stability is good, ultralow temperature control
Heat exchange efficiency is high, simple to operate, and automaticity is high.High compared with batch reaction yield and purity, stable reaction, side reaction is few, instead
Shorten between seasonable, it is most important that safe coefficient is high, by the near minimum point of potential safety hazard.Furthermore also there is small investment, take up an area face
The small advantage of product.
Further illustrate the beneficial effect of the application below in conjunction with specific embodiments.
Carried out respectively using the batch reactor of the continuous still reaction device shown in the application Fig. 1 and routine following anti-
Should, specific reaction equation is as follows：
Reaction effect see the table below 1.
Table 1：
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：
1. the production in enormous quantities application of n-BuLi participation can be realized using continuous still reaction device, n-BuLi
Treating capacity is up to the 1.5T/ months.
2. carrying out the production of butyl lithium using continuous still reaction device, according to reaction requirement series can be selected to carry out flexible
Combination, slave unit height and the consideration of floor space angle, preferably no greater than 6 grades.
3. carrying out the production of high-volume butyl lithium using continuous still reaction device, n-BuLi can be dilute in first order kettle
Release, two level kettle proceeds by reaction, and heat release is uniform, and safety coefficient is high.
4. each successive reaction kettle of design, the overflow volume maximum 14L of one-pot, material storage is few, material from leakage occurs
Disposable, hazards are small.
5. the successive reaction kettle of the application per one-level in reaction effect tracking it is convenient, intermediate detection occur it is abnormal, can be with
Regulation relevant feedstocks parameter in real time, be not in the phenomenon of high-volume material damage.
6. each successive reaction kettle carries agitating device, good mixing effect, reaction stability is good, product yield and purity
It is high.
7. the successive reaction kettle of the application uses the temperature control method of external jacket+inner coil pipe, temperature control heat transfer efficiency is high, for super
Low-temp reaction (<- 60 DEG C) it is especially suitable.
8. a whole set of continuous still reaction device can use the PLC control program of autonomous Design, each material charging can basis
Reaction result is flexibly set, and temperature and pressure parameter can detect in real time, has again ensured that the security of production；In addition, automatically control saving
Substantial amounts of manpower and materials.
9. in the application, the charging of each material uses the pipeline form in tubule (6~12mm) footpath, materials inside storage
Measure small, continuous safety in operation and stability height.
10. using 4 grades of continuous still reaction devices, the batch reactor relative to a 3000L compares, floor space
Small, equipment investment is few.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (17)
1. a kind of continuous still reaction device, it is characterised in that the continuous still reaction device includes：
N number of successive reaction kettle (10) for being sequentially connected in series setting, each successive reaction kettle (10) include body (11), described
Body (11) has reaction chamber (111), charging aperture (112), overfall (113) and discharging opening (114)；Wherein, N is oneself of >=2
So number, the charging aperture of the overfall (113) and successive reaction kettle (10) described in n-th of the N-1 successive reaction kettles (10)
(112) it is connected.
2. continuous still reaction device according to claim 1, it is characterised in that the N-1 successive reaction kettles
(10) overfall (113) is connected with the charging aperture (112) of successive reaction kettle (10) described in n-th by overflow passage.
3. continuous still reaction device according to claim 1, it is characterised in that the overfall (113) with it is described
Charging aperture (112) is sequentially connected on logical direction, and the overfall (113) of the N-1 successive reaction kettles (10) is higher than n-th
The charging aperture (112) of the successive reaction kettle (10).
4. continuous still reaction device according to claim 1, it is characterised in that multiple successive reaction kettle (10) water
It is flat to set, and it is provided with successive reaction kettle described in gas atmosphere inlet or n-th on first successive reaction kettle (10)
(10) vacuum extractor is provided with.
5. continuous still reaction device according to any one of claim 1 to 4, it is characterised in that the successive reaction
Kettle (10) also includes agitating device (12), and the agitating device (12) includes puddler and agitating paddle, and the agitating paddle is located at institute
State in reaction chamber (111), one end of the puddler is connected with the agitating paddle, and the other end extends to the body (11) outside simultaneously
It is connected with motor.
6. continuous still reaction device according to any one of claim 1 to 4, it is characterised in that the successive reaction
Kettle (10) also includes reacting kettle jacketing (13), and the reacting kettle jacketing (13) is set around the outer wall of each body (11).
7. continuous still reaction device according to claim 6, it is characterised in that the two neighboring successive reaction kettle
(10) reacting kettle jacketing (13) is connected corresponding to.
8. continuous still reaction device according to any one of claim 1 to 4, it is characterised in that the successive reaction
Kettle (10) also includes cooling coil (14), and the cooling coil (14) is arranged in the reaction chamber (111), and around described
The inwall of body (11) is set.
9. continuous still reaction device according to claim 8, it is characterised in that the two neighboring successive reaction kettle
(10) cooling coil (14) is connected corresponding to.
10. continuous still reaction device according to any one of claim 1 to 4, it is characterised in that the successive reaction
Kettle (10) also includes monitoring element and holds the sleeve pipe (15) of the monitoring element, and described sleeve pipe (15) passes through the body
(11) stretch into the reaction chamber (111).
11. continuous still reaction device according to claim 10, it is characterised in that the monitoring element be electroheat pair,
Thermal resistance and/or thermometer.
12. continuous still reaction device according to any one of claim 1 to 4, it is characterised in that the successive reaction
Kettle (10) also includes pressure transmitter (16), and the body (11) also includes the pressure through hole being arranged on roof, the pressure
Transmitter (16) is connected and is arranged on the outer wall of the body (11) with the pressure through hole.
13. a kind of n-BuLi participates in the continuous still reaction system of production, it is characterised in that the continuous still reaction system
Including：
Continuous still reaction device (01), the continuous still reaction device (01) is any one of claim 1 to 12
Continuous still reaction device；And
Feeding device (02), the feeding device (02) are connected with the charging aperture (112) of the continuous still reaction device (01)
It is logical.
14. continuous still reaction system according to claim 13, it is characterised in that the continuous still reaction system is also
Including：
Control device (03), the control device (03) are connected with the feeding device (02) to control the feeding device (02)
Feed quantity.
15. continuous still reaction system according to claim 14, it is characterised in that the control device (03) also with institute
State continuous still reaction device (01) to be connected, to monitor the running status of the continuous still reaction device (01), and described
Stop the feed of the feeding device (02) during continuous still reaction device (01) operation exception.
16. continuous still reaction system according to claim 14, it is characterised in that the feeding device (02) includes：
Feedstock storage unit (021)；
Metering device (022), the feedstock storage unit (021) are placed on the metering device (022), the metering device
(022) it is connected with the control device (03) so that the metric results are fed back into the control device (03)；
Feed pump (023), the feedstock storage unit (021) are filled by the feed pump (023) and the continuous still reaction
Put (01) to be connected, the feed pump (023) is connected with the control device (03) to control institute by the control device (03)
State the inlet amount of feed pump (023).
17. continuous still reaction system according to claim 16, it is characterised in that the feedstock storage unit (021)
Including nitrogen blow valve port (020), the continuous still reaction system also includes：
Product collecting device (04), the product collecting device (04) are arranged under the continuous still reaction device (01)
Trip；The nitrogen blow valve port (020) is connected with the control device (03), for after charging terminates, being filled by the control
Put (03) opening nitrogen blow valve port (020) reaction product is blown in the product collecting device (04).
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| CN201710675542.2A CN107537423A (en) | 2017-08-09 | 2017-08-09 | Continuous still reaction device and n-BuLi participate in the continuous still reaction system of production |
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| CN110194725A (en) * | 2018-02-26 | 2019-09-03 | 北京颖泰嘉和生物科技股份有限公司 | A kind of device and method of the continuous autoclave production imines of modified |
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| CN112500391A (en) * | 2020-12-14 | 2021-03-16 | 江西禾益化工股份有限公司 | Device and method for producing dithianon through continuous kettle type reaction |
| CN113856579A (en) * | 2021-08-16 | 2021-12-31 | 纽威科技(长沙)有限公司 | Heat exchange process and system for treating liquid substance |
| CN114539076A (en) * | 2022-03-28 | 2022-05-27 | 苏州市晶协高新电子材料有限公司 | Continuous synthesis device and process of dimethyl diallyl ammonium chloride |
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| CN114539076A (en) * | 2022-03-28 | 2022-05-27 | 苏州市晶协高新电子材料有限公司 | Continuous synthesis device and process of dimethyl diallyl ammonium chloride |
| CN116284060A (en) * | 2023-05-22 | 2023-06-23 | 研峰科技(北京)有限公司 | Safe production process of organic lithium reagent butyl lithium |
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