CN109503522A - A kind of tubular reactor of 3- hydroxyl tetrahydrofuran - Google Patents
A kind of tubular reactor of 3- hydroxyl tetrahydrofuran Download PDFInfo
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- CN109503522A CN109503522A CN201811608571.8A CN201811608571A CN109503522A CN 109503522 A CN109503522 A CN 109503522A CN 201811608571 A CN201811608571 A CN 201811608571A CN 109503522 A CN109503522 A CN 109503522A
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- sodium borohydride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/04—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D307/18—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/20—Oxygen atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the production technical fields of medicine intermediate, and in particular to a kind of tubular reactor of 3- hydroxyl tetrahydrofuran, comprising: storage device, the storage device include malic acid solution material-compound tank and sodium borohydride suspension formulations tank；Controllable type charging gear, the controllable type charging gear include PLC controller, rear pump and the flowmeter of signal connection, have signal input part and signal output end in the PLC controller；Controllable type charging gear is equipped on the output channel of malic acid solution material-compound tank and sodium borohydride suspension formulations tank, pass through the control to material rate and amount, it avoids using excessive sodium borohydride, to reduce the consumption of sodium borohydride, also hydrogen is avoided to cause security risk, it is placed in water bath, it is entered after material mixing in reaction helix tube, environment temperature is rapidly increased to reaction temperature, the fast reaction of material may be implemented, the variation for reducing integrated environment temperature guarantees that the safety and stability of reaction carries out.
Description
Technical field
The invention belongs to the production technical fields of medicine intermediate, and in particular to a kind of tubular type of 3- hydroxyl tetrahydrofuran is anti-
Answer device.
Background technique
3- hydroxyl tetrahydrofuran is using more and more in medical product, and wherein S-3- hydroxyl tetrahydrofuran downstream is main
Product has fosamprenavir (treatment for AIDS), and En Gelie is net (treatment for diabetes), Afatinib (anticarcinogen),
R-3- hydroxyl tetrahydrofuran (treatment for pfize alzheimer's disease), it can be seen that, 3- hydroxyl tetrahydrofuran is a kind of
Multiduty intermediate, with the listing of these drugs, the demand to 3- hydroxyl tetrahydrofuran can also expand.
However there are impassable limiting factors in existing production technology, currently, from apple dimethyl phthalate through
It crosses NaBH4 and restores to obtain 1,2,4-butanetriol and autoclave intermittence is all used to react, to guarantee reaction thoroughly, used in technique big
Big excessive sodium borohydride, methanol as reaction dissolvent at normal temperature to the decomposition rate of sodium borohydride quickly, not only consumption of boron
Sodium hydride also decomposes a large amount of hydrogen of generation and causes security risk；Reaction solution is added in sodium borohydride using under low temperature in technique
It is mixed with apple dimethyl phthalate, then is warming up to reaction temperature, since reduction reaction is the reaction of very exothermic, keep reaction temperature anxious
Play increases, and temperature further speeds up reaction speed after increasing, to further release a large amount of heat, forms vicious circle, reaction
It faces out of control；However optimal reaction temperature of this reaction is at 60-65 DEG C, excessive temperature is more than methanol boiling point, at slug, very
To Fire explosion；Reaction temperature is too low, and reaction is not thorough, at waste material；So in order to control risk, reaction can only small lot it is more
Batch carries out, and greatly limits the performance of production capacity；Nevertheless, every batch reaction all enables operator soul-stirring.
Summary of the invention
To solve the problems mentioned above in the background art.The present invention provides a kind of tubular type of 3- hydroxyl tetrahydrofuran is anti-
Device is answered, has the characteristics that small occupied area, continuous reaction, yield are big, safely controllable, fireballing.
To achieve the above object, the invention provides the following technical scheme: a kind of tubular reactor of 3- hydroxyl tetrahydrofuran,
It include: storage device, the storage device includes malic acid solution material-compound tank and sodium borohydride suspension formulations tank；Controllable type is given
Expect that device, the controllable type charging gear include PLC controller, rear pump and the flowmeter of signal connection, the PLC controller
Upper have signal input part and a signal output end, the rear pump and flowmeter be installed in the malic acid solution material-compound tank and
On the conveying pipeline of sodium borohydride suspension formulations tank, the output end of the flowmeter is connected on the signal input part, described
The output end of rear pump is connected on the signal output end；Mixing arrangement, the mixing arrangement includes material mixer, described
Material mixer is connected to the end of the malic acid solution material-compound tank and sodium borohydride suspension formulations tank conveying pipeline；Reaction dress
It sets, the reaction unit includes water bath and reaction helix tube, and the reaction helix tube is placed in the inside of the water bath, described
The output end of material mixer is connected on the reaction helix tube；Collection device, the collection device is to receive kettle, described anti-
Helix tube is answered to be connected to the input port for receiving kettle.
In order to can control output flow, as a preferred technical solution of the present invention, the rear pump and flowmeter
Quantity be two, a rear pump and flowmeter are connected in series in the conveying pipeline of the malic acid solution material-compound tank
On, and cooperate the flow closed-loop control system of the PLC controller composition malic acid solution material-compound tank, another described rear pump
It is connected in series in flowmeter on the conveying pipeline of the sodium borohydride suspension formulations tank, and the PLC controller is cooperated to form
The flow closed-loop control system of sodium borohydride suspension formulations tank.
In order to enable control output revolution speed, as a preferred technical solution of the present invention, the input of the rear pump
End is connected with frequency converter, and output signal is input in the frequency converter by the PLC controller by signal output end.
Putty in order to prevent, as a preferred technical solution of the present invention, the material mixer is SK type mixer.
In order to enable guaranteeing that water-bath is evenly heated, as a preferred technical solution of the present invention, the water bath is in cylinder
The bottom middle position of shape, the water bath has heating chamber, and the inner wall of the heating chamber is fixed with equally distributed electric heating
Element.
Bath temperature is carried out automatically controlling in order to realize, as a preferred technical solution of the present invention, the electric heating
Element is heating wire group, and temperature sensor is equipped in the water bath, and the temperature sensor and heating wire group are electrically connected.
For the ease of carrying out pressure control to bath temperature, as a preferred technical solution of the present invention, the water-bath
The top of case has water inlet, and the bottom of the water bath has discharge outlet.
In order to provide good reaction temperature atmosphere, as a preferred technical solution of the present invention, the reaction spiral
Pipe is spirally distributed in the water bath, and is located at the outside of the heating chamber, and the both ends of the reaction helix tube have
Input pipe and efferent duct, the input pipe are connected to the output end of the material mixer, and the efferent duct is connected to described connect
It receives on kettle.
Putty in order to prevent, as a preferred technical solution of the present invention, the inner wall smooth of the reaction helix tube.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention gives on the output channel of malic acid solution material-compound tank and sodium borohydride suspension formulations tank equipped with controllable type
Material device is avoided by the control to material rate and amount using excessive sodium borohydride, to reduce the consumption of sodium borohydride
Amount, it is thus also avoided that generate a large amount of hydrogen and cause security risk.
2, the present invention is equipped with reaction helix tube, is placed in water bath, is entered in reaction helix tube after material mixing, ring
Border temperature is rapidly increased to reaction temperature, the fast reaction of material may be implemented, and water has biggish specific heat capacity, can be to anti-
The heat answered is absorbed, and Spreading and diffusion, reduces the variation of integrated environment temperature, guarantees that the safety and stability of reaction carries out.
3, the present invention has the feeding of controllable automation and cooperates suitable reaction temperature, has continuous reaction, produces
Big, safely controllable and fireballing feature is measured, big progress is brought to production and processing.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is the mass flow closed-loop control schematic diagram in the present invention；
Fig. 3 is the water bath structural schematic diagram in the present invention；
In figure: 1, malic acid solution material-compound tank；2, sodium borohydride suspension formulations tank；3, PLC controller；31, signal input part；
32, signal output end；4, rear pump；5, flowmeter；6, material mixer；7, water bath；701, heating chamber；71, heating element；
72, water inlet；73, discharge outlet；8, helix tube is reacted；81, input pipe；82, efferent duct；9, kettle is received.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment
Fig. 1-3 is please referred to, the present invention provides a kind of technical solution: a kind of tubular reactor of 3- hydroxyl tetrahydrofuran, packet
Include: storage device, storage device include malic acid solution material-compound tank 1 and sodium borohydride suspension formulations tank 2；Controllable type feed dress
It sets, controllable type charging gear includes PLC controller 3, rear pump 4 and the flowmeter 5 of signal connection, has letter in PLC controller 3
Number input terminal 31 and signal output end 32, rear pump 4 and flowmeter 5 are installed in malic acid solution material-compound tank 1 and sodium borohydride
On the conveying pipeline of suspension formulations tank 2, the output end of flowmeter 5 is connected on signal input part 31, and the output end of rear pump 4 connects
It connects on signal output end 32；Mixing arrangement, mixing arrangement include material mixer 6, and it is molten that material mixer 6 is connected to malic acid
The end of 2 conveying pipeline of liquid material-compound tank 1 and sodium borohydride suspension formulations tank；Reaction unit, reaction unit include water bath 7 and anti-
Helix tube 8 is answered, reaction helix tube 8 is placed in the inside of water bath 7, and the output end of material mixer 6 is connected to reaction helix tube 8
On；Collection device, collection device are to receive kettle 9, and reaction helix tube 8 is connected to the input port for receiving kettle 9.
In the present embodiment, apple dimethyl phthalate material-compound tank 1, sodium borohydride material-compound tank 2 pass through the output of two sets of frequency control
4 control output flow of pump, rear pump 4 are followed by flowmeter 5, and flow signal is sent in PLC controller 3,3 basis of PLC controller
The frequency converter of changes in flow rate two rear pumps 4 of countercharge, adjusts frequency stabilization flow, realizes closed-loop control；The object of two rear pumps 4
Expect to carry out adequately being mixed into reaction helix tube 8 in the SK type mixer of setting after threeway, reaction helix tube 8 is placed in
In the water-bath of water bath 7, temperature of charge is rapidly increased to reaction temperature, fast reaction；Reaction helix tube 8 is designed as disc disk
Pipe, inner wall pass through polishing treatment, can reduce the resistance of ducting, solid material is avoided to adhere to；Reaction liquid stops 1-5 points in pipeline
Clock, access receive in kettle 9.
Specifically, the quantity of rear pump 4 and flowmeter 5 is two, a rear pump 4 and flowmeter 5 are connected in series in
On the conveying pipeline of malic acid solution material-compound tank 1, and cooperate the flow closed loop control of the composition malic acid solution material-compound tank 1 of PLC controller 3
System processed, another rear pump 4 and flowmeter 5 are connected in series on the conveying pipeline of sodium borohydride suspension formulations tank 2, and are cooperated
The flow closed-loop control system of the composition sodium borohydride suspension formulations tank 2 of PLC controller 3.
In the present embodiment, the quantity of rear pump 4 and flowmeter 5 is two, and a rear pump 4 and the series connection of flowmeter 5 connect
It connects on the conveying pipeline of malic acid solution material-compound tank 1, and the flow for cooperating PLC controller 3 to form malic acid solution material-compound tank 1 closes
Ring control system, another rear pump 4 and flowmeter 5 are connected in series on the conveying pipeline of sodium borohydride suspension formulations tank 2, and
PLC controller 3 is cooperated to form the flow closed-loop control system of sodium borohydride suspension formulations tank 2, malic acid solution material-compound tank 1
The closed-loop control system to flow control is separately configured on the conveying pipeline of conveying pipeline and sodium borohydride suspension formulations tank 2,
Detect that the flow signal in pipeline is sent in PLC controller 3 by flowmeter 5, PLC controller 3 is anti-according to changes in flow rate
The frequency converter of two rear pumps 4 is controlled, frequency stabilization flow is adjusted, realizes closed-loop control.
Specifically, the input terminal of rear pump 4 is connected with frequency converter, PLC controller 3 is believed output by signal output end 32
It number is input in frequency converter.
In the present embodiment, the input terminal of rear pump 4 is connected with frequency converter, and PLC controller 3 will be defeated by signal output end 32
Signal is input in frequency converter out, the revolving speed of the power control rear pump 4 by controlling frequency converter, to realize to uninterrupted
It is controlled.
Specifically, material mixer 6 is SK type mixer.
In the present embodiment, material mixer 6 is SK type mixer, and SK type static mixer is suitable for requiring less high mix
Conjunction process can be used for augmentation of heat transfer, and SK type is least easy blocking in the static mixer of various models.
Specifically, water bath 7 is cylindrical in shape, the bottom middle position of water bath 7 has heating chamber 701, heating chamber 701
Inner wall is fixed with equally distributed heating element 71.
In the present embodiment, water bath 7 is cylindrical in shape, and the bottom middle position of water bath 7 has heating chamber 701, heating chamber
701 inner wall is fixed with equally distributed heating element 71, may be implemented rapidly and uniformly to heat the water in water bath 7.
Specifically, heating element 71 is heating wire group, temperature sensor, temperature sensor and electric heating are equipped in water bath 7
Silk group is electrically connected.
In the present embodiment, heating element 71 is heating wire group, is equipped with temperature sensor in water bath 7, temperature sensor with
Heating wire group is electrically connected, and is fed back by temperature sensor to the water temperature in water bath 7, and the heating of heating element 71 is controlled
Power, and then control water temperature.
Specifically, the top of water bath 7 has water inlet 72, the bottom of water bath 7 has discharge outlet 73.
In the present embodiment, the top of water bath 7 has water inlet 72, and the bottom of water bath 7 has discharge outlet 73, Ke Yigen
According to the water temperature in water bath 7, by water inlet 72 and discharge outlet 73 forces that cooling water is added, be used for balanced reaction temp.
Specifically, reaction helix tube 8 is spirally distributed in water bath 7, and it is located at the outside of heating chamber 701, reaction
The both ends of helix tube 8 have input pipe 81 and efferent duct 82, and input pipe 81 is connected to the output end of material mixer 6, efferent duct
82 are connected on reception kettle 9.
In the present embodiment, reaction helix tube 8 is spirally distributed in water bath 7, and is located at the outside of heating chamber 701,
Guarantee reaction 8 thermally equivalent of helix tube, the both ends of reaction helix tube 8 have input pipe 81 and efferent duct 82, and input pipe 81 connects
In the output end of material mixer 6, efferent duct 82, which is connected to, to be received on kettle 9.
Specifically, the inner wall smooth of reaction helix tube 8.
In the present embodiment, the inner wall smooth of helix tube 8 is reacted, the resistance of ducting can be reduced, solid material is avoided to adhere to.
The working principle of the invention and process for using: after the present invention installs, apple dimethyl phthalate material-compound tank 1, boron hydrogen
Change sodium material-compound tank 2 and output flow is controlled by the rear pump 4 of two sets of frequency control, rear pump 4 is followed by flowmeter 5, flow signal
It is sent in PLC controller 3, PLC controller 3 adjusts frequency stabilization according to the frequency converter of changes in flow rate two rear pumps 4 of countercharge
Flow realizes closed-loop control；It by the control to material rate and amount, avoids using excessive sodium borohydride, to reduce boron
The consumption of sodium hydride, it is thus also avoided that generate a large amount of hydrogen and cause security risk, the material of two rear pumps 4 is after threeway
It carries out adequately being mixed into reaction helix tube 8 in the SK type mixer of setting, reaction helix tube 8 is placed in the water of water bath 7
In bath, environment temperature is rapidly increased to reaction temperature, the fast reaction of material may be implemented, and water has biggish specific heat capacity,
The heat of reaction can be absorbed, and Spreading and diffusion, reduce integrated environment temperature variation, guarantee reaction safety and stability into
Row, reaction helix tube 8 are designed as disc coil pipe, and inner wall passes through polishing treatment, can reduce the resistance of ducting, avoid solid material attached
?；Reaction liquid stops 1-5 minutes in pipeline, and access receives in kettle 9.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (9)
1. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran, it is characterised in that: include:
Storage device, the storage device include malic acid solution material-compound tank (1) and sodium borohydride suspension formulations tank (2)；
Controllable type charging gear, the controllable type charging gear include PLC controller (3), rear pump (4) and the stream of signal connection
Meter (5), has signal input part (31) and signal output end (32) on the PLC controller (3), the rear pump (4) and
Flowmeter (5) is installed on the conveying pipeline of the malic acid solution material-compound tank (1) and sodium borohydride suspension formulations tank (2),
The output end of the flowmeter (5) is connected on the signal input part (31), and the output end of the rear pump (4) is connected to institute
It states on signal output end (32)；
Mixing arrangement, the mixing arrangement include material mixer (6), and the material mixer (6) is connected to the malic acid
The end of solution material-compound tank (1) and sodium borohydride suspension formulations tank (2) conveying pipeline；
Reaction unit, the reaction unit include water bath (7) and reaction helix tube (8), and the reaction helix tube (8) is placed in institute
The inside of water bath (7) is stated, the output end of the material mixer (6) is connected on the reaction helix tube (8)；
Collection device, the collection device are to receive kettle (9), and reaction helix tube (8) is connected to the defeated of reception kettle (9)
Entrance.
2. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the rear pump
(4) and the quantity of flowmeter (5) is two, and a rear pump (4) and flowmeter (5) are connected in series in the malic acid
On the conveying pipeline of solution material-compound tank (1), and the flow of the PLC controller (3) composition malic acid solution material-compound tank (1) is cooperated to close
Ring control system, another described rear pump (4) and flowmeter (5) are connected in series in the sodium borohydride suspension formulations tank
(2) on conveying pipeline, and cooperate the flow closed-loop control of the PLC controller (3) composition sodium borohydride suspension formulations tank (2)
System.
3. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the rear pump
(4) input terminal is connected with frequency converter, and output signal is input to institute by signal output end (32) by the PLC controller (3)
It states in frequency converter.
4. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the material is mixed
Clutch (6) is SK type mixer.
5. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the water bath
(7) it is cylindrical in shape, the bottom middle position of the water bath (7) has heating chamber (701), the inner wall of the heating chamber (701)
It is fixed with equally distributed heating element (71).
6. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 5, it is characterised in that: the electric heating member
Part (71) is heating wire group, is equipped with temperature sensor in the water bath (7), the temperature sensor electrically connects with heating wire group
It connects.
7. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the water bath
(7) top has water inlet (72), and the bottom of the water bath (7) has discharge outlet (73).
8. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 6, it is characterised in that: the reaction spiral shell
Coil (8) is spirally distributed in the water bath (7), and is located at the outside of the heating chamber (701), the reaction spiral
The both ends for managing (8) have input pipe (81) and efferent duct (82), and the input pipe (81) is connected to the material mixer (6)
Output end, the efferent duct (82) are connected on the reception kettle (9).
9. a kind of tubular reactor of 3- hydroxyl tetrahydrofuran according to claim 1, it is characterised in that: the reaction spiral shell
The inner wall smooth of coil (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811608571.8A CN109503522A (en) | 2018-12-27 | 2018-12-27 | A kind of tubular reactor of 3- hydroxyl tetrahydrofuran |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811608571.8A CN109503522A (en) | 2018-12-27 | 2018-12-27 | A kind of tubular reactor of 3- hydroxyl tetrahydrofuran |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644116A (en) * | 2020-04-30 | 2020-09-11 | 兰州兰石中科纳米科技有限公司 | Batching device |
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| CN107235937A (en) * | 2017-07-12 | 2017-10-10 | 海门华祥医药科技有限公司 | A kind of synthetic method of (S) 3 hydroxyl tetrahydrofuran |
| CN108554361A (en) * | 2018-01-08 | 2018-09-21 | 江苏三江机电工程有限公司 | Tubular continuous reactor |
| CN108774209A (en) * | 2018-08-03 | 2018-11-09 | 苏州富士莱医药股份有限公司 | A method of lipoic acid ethyl ester is prepared using tubular reactor |
| CN209481521U (en) * | 2018-12-27 | 2019-10-11 | 江苏联昇化学有限公司 | A kind of tubular reactor of 3- hydroxyl tetrahydrofuran |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644116A (en) * | 2020-04-30 | 2020-09-11 | 兰州兰石中科纳米科技有限公司 | Batching device |
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