CN209481521U - A kind of tubular reactor of 3- hydroxyl tetrahydrofuran - Google Patents

A kind of tubular reactor of 3- hydroxyl tetrahydrofuran Download PDF

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Publication number
CN209481521U
CN209481521U CN201822212145.4U CN201822212145U CN209481521U CN 209481521 U CN209481521 U CN 209481521U CN 201822212145 U CN201822212145 U CN 201822212145U CN 209481521 U CN209481521 U CN 209481521U
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China
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reaction
sodium borohydride
tank
water bath
tubular reactor
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Expired - Fee Related
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CN201822212145.4U
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Chinese (zh)
Inventor
夏冬前
肖冬子
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Jiangsu Airy Chemical Co ltd
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Jiangsu Shenghua Chemical Co Ltd
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Abstract

The utility model belongs to the production technical field 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

A kind of tubular reactor of 3- hydroxyl tetrahydrofuran
Technical field
The utility model belongs to the production technical field of medicine intermediate, and in particular to a kind of pipe of 3- hydroxyl tetrahydrofuran Formula reactor.
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.
Utility model content
To solve the problems mentioned above in the background art.The utility model provides a kind of pipe of 3- hydroxyl tetrahydrofuran Formula reactor has the characteristics that small occupied area, continuous reaction, yield are big, safely controllable, fireballing.
To achieve the above object, the utility model provides the following technical solutions: a kind of tubular type of 3- hydroxyl tetrahydrofuran is anti- Answer device, comprising: storage device, the storage device include malic acid solution material-compound tank and sodium borohydride suspension formulations tank;It can Control formula charging gear, the controllable type charging gear include PLC controller, rear pump and the flowmeter of signal connection, the PLC There is signal input part and signal output end, the rear pump and flowmeter are installed in the malic acid solution and match on controller On the conveying pipeline of batch can and sodium borohydride suspension formulations tank, the output end of the flowmeter is connected to the signal input part On, the output end of the rear pump is connected on the signal output end;Mixing arrangement, the mixing arrangement include material mixing Device, the material mixer are connected to the end of the malic acid solution material-compound tank and sodium borohydride suspension formulations tank conveying pipeline End;Reaction unit, the reaction unit include water bath and reaction helix tube, and the reaction helix tube is placed in the water bath Inside, the output end of the material mixer are connected on the reaction helix tube;Collection device, the collection device are to receive Kettle, the reaction helix tube are connected to the input port for receiving kettle.
In order to can control output flow, as a kind of optimal technical scheme of the utility model, the rear pump and stream The quantity of meter is two, and a rear pump and flowmeter are connected in series in the conveying of the malic acid solution material-compound tank Guan Shang, and cooperate the flow closed-loop control system of the PLC controller composition malic acid solution material-compound tank, another described output Pump and flowmeter are connected in series on the conveying pipeline of the sodium borohydride suspension formulations tank, and cooperate the PLC controller group At the flow closed-loop control system of sodium borohydride suspension formulations tank.
In order to enable control output revolution speed, as a kind of optimal technical scheme of the utility model, the rear pump Input terminal 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 kind of optimal technical scheme of the utility model, the material mixer is mixed for SK type Clutch.
In order to enable guaranteeing that water-bath is evenly heated, as a kind of optimal technical scheme of the utility model, the water bath It is cylindrical in shape, the bottom middle position of the water bath has heating chamber, and the inner wall of the heating chamber is fixed with equally distributed Heating element.
Bath temperature is carried out automatically controlling in order to realize, it is described as a kind of optimal technical scheme of the utility model Heating element is heating wire group, is equipped with temperature sensor in the water bath, the temperature sensor electrically connects with heating wire group It connects.
It is described as a kind of optimal technical scheme of the utility model for the ease of carrying out pressure control to bath temperature The top of water bath has water inlet, and the bottom of the water bath has discharge outlet.
In order to provide good reaction temperature atmosphere, as a kind of optimal technical scheme of the utility model, the reaction Helix tube is spirally distributed in the water bath, and is located at the outside of the heating chamber, the both ends of the reaction helix tube With input pipe and efferent duct, the input pipe is connected to the output end of the material mixer, and the efferent duct is connected to institute It states and receives on kettle.
Putty in order to prevent, as a kind of optimal technical scheme of the utility model, the inner wall light of the reaction helix tube It is sliding.
Compared with prior art, the utility model has the beneficial effects that
1, the utility model is equipped on the output channel of malic acid solution material-compound tank and sodium borohydride suspension formulations tank Controllable type charging gear is avoided by the control to material rate and amount using excessive sodium borohydride, to reduce hydroboration The consumption of sodium, it is thus also avoided that generate a large amount of hydrogen and cause security risk.
2, the utility model is equipped with reaction helix tube, is placed in water bath, enters reaction helix tube after material mixing In, environment temperature is rapidly increased to reaction temperature, the fast reaction of material may be implemented, and water has biggish specific heat capacity, can To absorb to the heat of reaction, and Spreading and diffusion, reduce the variation of integrated environment temperature, guarantee the safety and stability of reaction into Row.
Detailed description of the invention
Attached drawing is used to provide a further understanding of the present invention, and constitutes part of specification, practical with this Novel embodiment is used to explain the utility model together, does not constitute limitations of the present invention.In the accompanying drawings:
Fig. 1 is the structural schematic diagram of the utility model;
Fig. 2 is the mass flow closed-loop control schematic diagram in the utility model;
Fig. 3 is the water bath structural schematic diagram in the utility model;
In figure: 1, malic acid solution material-compound tank;2, sodium borohydride suspension formulations tank;3, PLC controller;31, signal is defeated Enter end;32, signal output end;4, rear pump;5, flowmeter;6, material mixer;7, water bath;701, heating chamber;71, electric 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
The following will be combined with the drawings in the embodiments of the present invention, carries out the technical scheme in the embodiment of the utility model Clearly and completely describe, it is clear that the described embodiments are only a part of the embodiments of the utility model, rather than whole Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are without making creative work Every other embodiment obtained, fall within the protection scope of the utility model.
Embodiment
Fig. 1-3 is please referred to, the utility model provides a kind of technical solution: a kind of pipe reaction of 3- hydroxyl tetrahydrofuran Device, comprising: storage device, storage device include malic acid solution material-compound tank 1 and sodium borohydride suspension formulations tank 2;Controllable type Charging gear, controllable type charging gear includes PLC controller 3, rear pump 4 and the flowmeter 5 of signal connection, in PLC controller 3 With signal input part 31 and signal output end 32, rear pump 4 and flowmeter 5 are installed in malic acid solution material-compound tank 1 and boron On the conveying pipeline of sodium hydride suspension formulations tank 2, the output end of flowmeter 5 is connected on signal input part 31, rear pump 4 it is defeated Outlet is connected on signal output end 32;Mixing arrangement, mixing arrangement include material mixer 6, and material mixer 6 is connected to apple The end of 2 conveying pipeline of tartaric acid solution material-compound tank 1 and sodium borohydride suspension formulations tank;Reaction unit, reaction unit include water-bath Case 7 and reaction helix tube 8, reaction helix tube 8 are placed in the inside of water bath 7, and the output end of material mixer 6 is connected to reaction spiral shell On coil 8;Collection device, collection device are to receive kettle 9, and reaction helix tube 8 is connected to the input port for receiving kettle 9.
Specifically, apple dimethyl phthalate material-compound tank 1, sodium borohydride material-compound tank 2 are controlled by the rear pump 4 of two sets of frequency control Output flow processed, rear pump 4 are followed by flowmeter 5, and flow signal is sent in PLC controller 3, and PLC controller 3 becomes according to flow Change the frequency converter of two rear pumps 4 of countercharge, adjust frequency stabilization flow, realizes closed-loop control;The material of two rear pumps 4 passes through It carries 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 water bath In 7 water-bath, temperature of charge is rapidly increased to reaction temperature, fast reaction;Reaction helix tube 8 is designed as disc coil pipe, inner wall By polishing treatment, the resistance of ducting can be reduced, solid material is avoided to adhere to;Reaction liquid stops 1-5 minutes in pipeline, access It receives 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 PLC controller 3 forms the flow closed-loop control system of sodium borohydride suspension formulations tank 2, the conveying of malic acid solution material-compound tank 1 The closed-loop control system to flow control is separately configured on the conveying pipeline of pipe and sodium borohydride suspension formulations tank 2, passes through Flowmeter 5 detects that the flow signal in pipeline is sent in PLC controller 3, and PLC controller 3 is according to changes in flow rate countercharge two The frequency converter of platform rear pump 4 adjusts frequency stabilization flow, 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, the revolving speed of the power control rear pump 4 by controlling frequency converter carries out uninterrupted to realize Control.
Specifically, material mixer 6 is SK type mixer, SK type static mixer is suitable for requiring less high mixing Journey 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, 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, and is fed back by temperature sensor to the water temperature in water bath 7, and the heating function of heating element 71 is controlled Rate, 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, can be according to water Water temperature in bath cabinet 7 by water inlet 72 and discharge outlet 73 forces that cooling water is added, is 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, guarantees 8 thermally equivalent of helix tube is reacted, the both ends of reaction helix tube 8 have input pipe 81 and efferent duct 82, and input pipe 81 is connected to object Expect the output end of 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, can reduce the resistance of ducting, solid material is avoided to adhere to.
The working principle and process for using of the utility model: after the utility model installs, apple dimethyl phthalate ingredient Tank 1, sodium borohydride material-compound tank 2 control output flow by the rear pump 4 of two sets of frequency control, and rear pump 4 is followed by flowmeter 5, Flow signal is sent in PLC controller 3, frequency converter of the PLC controller 3 according to changes in flow rate two rear pumps 4 of countercharge, adjustment Frequency stabilization flow realizes closed-loop control;By the control to material rate and amount, avoid using excessive sodium borohydride, from And reduce the consumption of sodium borohydride, it is thus also avoided that generate a large amount of hydrogen and cause security risk, the material warp of two rear pumps 4 It crosses and carries out after threeway being adequately mixed into reaction helix tube 8 in the SK type mixer of setting, reaction helix tube 8 is placed in water-bath In the water-bath of case 7, environment temperature is rapidly increased to reaction temperature, the fast reaction of material may be implemented, and water is with biggish Specific heat capacity can absorb the heat of reaction, and Spreading and diffusion, reduce the variation of integrated environment temperature, guarantee the peace of reaction Complete stablize carries out, and reaction helix tube 8 is designed as disc coil pipe, and inner wall passes through polishing treatment, can reduce the resistance of ducting, avoids solid The attachment of body material;Reaction liquid stops 1-5 minutes in pipeline, and access receives in kettle 9.
Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention, it is not limited to this Utility model, although the utility model is described in detail with reference to the foregoing embodiments, for those skilled in the art For, it is still possible to modify the technical solutions described in the foregoing embodiments, or to part of technical characteristic It is equivalently replaced.Within the spirit and principle of the utility model, any modification, equivalent replacement, improvement and so on, It should be included within the scope of protection of this utility model.

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).
CN201822212145.4U 2018-12-27 2018-12-27 A kind of tubular reactor of 3- hydroxyl tetrahydrofuran Expired - Fee Related CN209481521U (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109503522A (en) * 2018-12-27 2019-03-22 江苏联昇化学有限公司 A kind of tubular reactor of 3- hydroxyl tetrahydrofuran

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109503522A (en) * 2018-12-27 2019-03-22 江苏联昇化学有限公司 A kind of tubular reactor of 3- hydroxyl tetrahydrofuran

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Address after: 225400 No. 88 Qidong Road, Binjiang Town Economic Development Zone, Taixing City, Jiangsu Province

Patentee after: Jiangsu airy Chemical Co.,Ltd.

Address before: 225400 No. 88 Qidong Road, Binjiang Town Economic Development Zone, Taixing City, Jiangsu Province

Patentee before: JIANGSU LIANSHENG CHEMICAL Co.,Ltd.

CF01 Termination of patent right due to non-payment of annual fee
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Granted publication date: 20191011