CN114797739A - Pipeline reactor and method for synthesizing materials by using same - Google Patents
Pipeline reactor and method for synthesizing materials by using same Download PDFInfo
- Publication number
- CN114797739A CN114797739A CN202210600064.XA CN202210600064A CN114797739A CN 114797739 A CN114797739 A CN 114797739A CN 202210600064 A CN202210600064 A CN 202210600064A CN 114797739 A CN114797739 A CN 114797739A
- Authority
- CN
- China
- Prior art keywords
- gas
- reaction
- pipe
- stirring
- rotating shaft
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/08—Hydrazoic acid; Azides; Halogen azides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The technical scheme of the invention is realized as follows: a pipeline reactor comprises a tank body, a temperature control device is arranged in the tank body, and a heat transfer layer is arranged outside the tank body; the reaction tube is spirally wound outside the tank body; the dosing mechanism comprises a plurality of dosing units which are uniformly arranged around the circumferential direction of the tank body at intervals; the driving mechanism is used for controlling the dosing mechanism to simultaneously add gas materials into the reaction tubes at different heights outside the tank body in an interval mode; the reaction mechanism is used for reacting sulfuric acid, ethanol and sodium nitrite and storing the produced ethyl nitrite gas; a flip bucket is arranged on the inner wall of the reaction tube; the invention has the beneficial effects that: the reaction is uniformly mixed, and the reaction efficiency is high.
Description
Technical Field
The invention relates to the technical field of reaction devices, in particular to a pipeline reactor and a method for synthesizing materials by using the same.
Background
Sodium azide, also known as sodium nitride, of the chemical formula NaN3, is an inorganic compound, is a white hexagonal crystal, is tasteless, odorless, non-hygroscopic, highly toxic, insoluble in diethyl ether, sparingly soluble in ethanol, soluble in liquid ammonia and water. Although nonflammable, explosive. Can be gradually decomposed into metallic sodium and nitrogen gas without explosion when heated in vacuum, is one of laboratory manufacturing methods of high-purity metallic sodium, and is also high-purity N 2 One of the laboratory manufacturing methods. Reacting with acid to produce hydrogen azide acid. Sodium azide reacts with most alkaline earth metals, salts of monovalent or polyvalent heavy metals, and hydroxides to form azides. In particular, copper, lead, silver, brass, bronze, etc. react to form highly explosive heavy metal azides. Reaction with a reactive organic halide to form an unstable organic azide.
In the existing pipeline reactor for producing sodium azide, for example, the pipeline reactor disclosed in patent publication No. CN103551102B, as with most pipeline reactors in the existing market, needs to occupy a large floor space and is difficult to ensure the sufficient mixing reaction of materials.
Disclosure of Invention
In view of the shortcomings of the prior art, the present invention provides a pipeline reactor and a method for synthesizing materials thereof, which are used to solve the problems in the background art.
The technical scheme of the invention is realized as follows: a pipeline reactor, characterized by: comprises a tank body, a temperature control device is arranged in the tank body, and a heat transfer layer is arranged outside the tank body; the reaction tube is spirally wound outside the tank body; the dosing mechanism comprises a plurality of dosing units which are uniformly arranged around the circumferential direction of the tank body at intervals; the driving mechanism is used for controlling the dosing mechanism to simultaneously add gas materials into the reaction tubes with different heights outside the tank body at intervals; the reaction mechanism is used for reacting sulfuric acid, ethanol and sodium nitrite and storing the produced ethyl nitrite gas; and the inner wall of the reaction tube is provided with a flip bucket.
Through above-mentioned technical scheme, through with the reactor around establishing on jar body, then at the internal temperature regulating device that sets up of jar, it is convenient to control the temperature, is convenient for control the unification of the temperature of all reaction tubes, and when the mixture is carried, flows round the body, forms spiral rivers, and the mix of the material of being convenient for is chosen the setting of class bank simultaneously, and the material strikes when flowing and is chosen the class bank, produces the torrent, and the mix of the material of being convenient for flows, improves reaction efficiency.
Preferably, the following components are used: the dosing unit comprises a lifting rod, is vertically arranged outside the induction pipe and is controlled to lift by the driving mechanism; the feeding units are uniformly arranged at one end of the lifting rod close to the dosing mechanism, and the feeding units are arranged at different heights and respectively feed materials corresponding to the reaction tubes at one height; each feeding unit is communicated with the reaction mechanism.
Preferably: the feeding unit comprises a feeding pipe which is vertically arranged at the upper end of the reaction pipe, the lower end of the feeding pipe is inserted into the reaction pipe, and a feeding hole is formed in part of the side wall of the feeding pipe, which is positioned in the reaction pipe; the sealing sleeve is fixed in the reaction tube, wraps the side wall of the feeding tube and can seal the feeding hole of the feeding tube; the reset plate is positioned at the upper end of the feeding pipe and fixedly connected with the feeding pipe, and the reset plate is fixedly connected with the lifting rod; the first spring is arranged at the bottom of the reset plate, and two ends of the first spring are respectively and fixedly connected with the upper end of the reaction tube and the lower end of the reset plate; the feed pipe can pass in and out the sealing sleeve when moving up and down.
Preferably: the driving mechanism comprises a lifting disc which is positioned at the top of the tank body and is fixedly connected with each lifting rod; the supporting frame is arranged at the upper end of the lifting disc, and the bottom of the supporting frame extends downwards to pass through the lifting disc to be fixedly connected with the tank body; the second spring is arranged at the bottom of the support frame, and two ends of the second spring are respectively fixedly connected with the bottom of the support frame and the top of the lifting disc; the motor is arranged at the bottom of the lifting frame; the center of the turntable is fixedly connected with the output end of the motor and is controlled by the motor to rotate; and the convex teeth are fixed on the side wall at one end of the rotary disc and can be in contact with the lifting disc and can extrude and move the lifting disc downwards.
Preferably: the reaction mechanism comprises a reaction kettle for the reaction of sulfuric acid, ethanol and sodium nitrite; the gas storage tank is communicated with the reaction kettle through a first gas pipe, one end of the gas storage tank is provided with a second gas pipe, the second gas pipe is provided with a plurality of third gas pipes, and each third gas pipe is communicated with one feeding pipe; the piston is arranged in the air storage box; the electric push rod is arranged on one side of the piston, which is far away from the second gas transmission pipe, and the electric push rod is arranged on the inner wall of the gas storage box and used for controlling the movement of the piston; and the first air conveying pipe and the second air conveying pipe are both provided with one-way valves.
Preferably, the following components are used: the stirring mechanism comprises a mounting frame and is fixed on the inner bottom wall of the reaction tube; the first rotating shaft is horizontally arranged in the reaction tube and is rotatably arranged on the mounting frame through a bearing; the spiral stirring paddle is fixed on the first rotation; the transmission gear is fixed on the first rotating shaft; and the toothed bar is vertically arranged in the reaction tube and fixed at the bottom of the feeding tube, and the toothed bar is in meshing transmission with the transmission gear.
Preferably: the stirring mechanism also comprises a second rotating shaft which is vertically arranged in the reaction tube and is rotatably arranged on the mounting frame through a bearing; the first conical gear is fixed on the first rotating shaft; the second bevel gear is fixed on the second rotating shaft and is in meshing transmission with the first bevel gear; and the stirring unit is fixed on the second rotating shaft.
Preferably: the stirring unit comprises a stirring disc and is fixed on the second rotating shaft; the sliding grooves are circumferentially and uniformly formed in the lower end of the stirring plate, and the width of each sliding groove is gradually reduced from top to bottom; the sliding block is arranged in the sliding groove and can slide in the sliding groove; the stirring rod is vertically arranged at the bottom of the stirring disc, one end of the stirring rod extends upwards to penetrate through the sliding groove to be fixedly connected with the sliding block, and a balancing weight is fixed at the bottom of the stirring rod; the sliding groove gradually inclines upwards from the second rotating shaft to the direction far away from the second rotating shaft.
A method for synthesizing materials by using a pipeline reactor is suitable for the pipeline reactor and is characterized by comprising the following steps:
s1: preparing ethanol and sodium nitrite solution in a reaction kettle, adding sulfuric acid into the reaction kettle to mix with the solution consisting of ethanol and sodium nitrite, introducing ethyl nitrite gas generated in the reaction kettle into a gas storage tank through a first gas conveying pipe, closing a one-way valve on the first gas conveying pipe after the reaction is completed, opening a one-way valve on a second gas conveying pipe, pushing a piston through an electric push rod to extrude the ethyl nitrite gas into a feeding pipe, and maintaining the pressure value in the gas storage tank;
s2: adjusting a temperature control device in the tank body, controlling the temperature of a reaction tube to be 18-25 ℃, then preparing a mixture consisting of hydrazine hydrate, sodium hydroxide, a catalyst and ethanol to be input into the reaction tube, and enabling the mixture to spirally flow in the reaction tube and to be fully mixed in the reaction tube through the flip flow of the flip bucket;
s3; starting an electric motor to drive a turntable and convex teeth to rotate, wherein the convex teeth rotate downwards to extrude a lifting disc to drive the lifting disc and a lifting rod to move downwards, each feed pipe moves downwards to penetrate out of a sealing sleeve, a feed port on each feed pipe is opened to add ethyl nitrite gas into a reaction pipe, reaction pipes with different heights are simultaneously added with equal amounts of ethyl nitrite gas to be mixed with a mixture, the turntable continues to rotate, the convex teeth rotate upwards until the convex teeth do not contact with the lifting disc, the lifting rod and the feed pipes are driven to move upwards through the elasticity of a first spring and a second spring, the feed pipes enter the sealing sleeve, the feed ports are closed to stop adding gas, once gas is added into the reaction pipes every time the turntable rotates for one circle along with the rotation of the motor, and the gas is added into the reaction pipes intermittently to be mixed with the mixture;
s4: when the feeding pipe moves up and down, the toothed bar moves up and down along with the feeding pipe, the transmission gear is driven to rotate repeatedly in clockwise and anticlockwise directions, the first rotating shaft and the spiral stirring paddle are driven to rotate forward and turn over to drive a mixture and gas to be stirred and mixed, the first bevel gear rotates along with the first rotating shaft and drives the second bevel gear and the second rotating shaft to rotate, the stirring disc rotates along with the first rotating shaft, the sliding block and the stirring bar move towards one end far away from the second rotating shaft during rotation to drive the mixture to be stirred, after rotation is stopped, the sliding block and the stirring bar move towards the direction close to the rotating shaft, and the stirring bar moves repeatedly and rotates to stir and mix the mixture and the gas repeatedly in a stirring direction different from that of the spiral stirring paddle;
s5: and (3) reacting the mixture and gas in a reaction tube for 1-2 hours, introducing all the gas in the first half hour, then distilling the finally obtained reaction liquid under reduced pressure to recover ethanol, carrying out suction filtration to obtain a wet product, and then drying under reduced pressure to obtain a fixed product.
Preferably: the catalyst in step S2 is tributylamine.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a schematic cross-sectional view of an embodiment of the present invention;
FIG. 3 is a schematic diagram of the structure of a feed unit in an embodiment of the present invention;
FIG. 4 is a schematic structural view of a reaction mechanism according to an embodiment of the present invention;
FIG. 5 is a schematic structural view of a stirring mechanism according to an embodiment of the present invention;
FIG. 6 is a schematic cross-sectional view of a stir plate in accordance with an embodiment of the present invention;
the examples in the figure are:
1. a tank body;
2. a reaction tube; 21. a flip bucket; 22. a lifting rod;
3. a feed unit; 31. a feed pipe; 32. a feed inlet; 33. a sealing sleeve; 34. a reset plate; 35. a first spring;
4. a drive mechanism; 41. a lifting plate; 42. a support frame; 43. a second spring; 44. a motor; 45. a turntable; 46. a convex tooth;
5. a reaction mechanism; 51. a reaction kettle; 52. a gas storage tank; 53. a first gas delivery pipe; 54. a second gas delivery pipe; 55. a third gas delivery pipe; 56. a piston; 57. an electric push rod;
6. a stirring mechanism; 61. a mounting frame; 62. a first rotating shaft; 63. a helical stirring paddle; 64. a transmission gear; 65. a rack bar; 66. a second rotating shaft; 67. a first bevel gear; 68. a second bevel gear; 69. a stirring unit; 691. a stirring plate; 692. a sliding groove; 693. a slider; 694. a stirring rod; 695. and a balancing weight.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 1, the present invention discloses a pipeline reactor, which comprises a tank 1, a temperature control device disposed in the tank, and a heat transfer layer disposed outside the tank 1; the reaction tube 2 is spirally wound outside the tank body 1; the dosing mechanism comprises a plurality of dosing units which are uniformly arranged around the circumferential direction of the tank body 1 at intervals; the driving mechanism 4 is used for controlling the dosing mechanism to simultaneously feed gas materials into the reaction tubes 2 at different heights outside the tank body 1 at intervals; the reaction mechanism 5 is used for reacting sulfuric acid, ethanol and sodium nitrite and storing the produced ethyl nitrite gas; and a flip bucket 21 is arranged on the inner wall of the reaction tube 2.
Through above-mentioned technical scheme, through with the reactor around establishing on jar body, then at the internal temperature regulating device that sets up of jar, it is convenient to control the temperature, is convenient for control the unification of the temperature of all reaction tubes, and when the mixture is carried, flows round the body, forms spiral rivers, and the mix of the material of being convenient for is chosen the setting of class bank simultaneously, and the material strikes when flowing and is chosen the class bank, produces the torrent, and the mix of the material of being convenient for flows, improves reaction efficiency.
Example 2
As shown in fig. 1 to 4, in the present embodiment, the dosing unit includes a lifting rod 22 vertically disposed outside the induction tube, and the lifting action is controlled by the driving mechanism 4; the feeding units 3 are uniformly arranged at one end of the lifting rod 22 close to the dosing mechanism, and the feeding units 3 are arranged at different heights and respectively feed materials corresponding to the reaction tubes 2 at one height; each of the feed units 3 is communicated with the reaction mechanism 5.
In this embodiment, the feeding unit 3 includes a feeding pipe 31 vertically disposed at the upper end of the reaction tube 2, and the lower end of the feeding pipe is inserted into the reaction tube 2, and a feeding port 32 is opened on a portion of the side wall of the feeding pipe 31 located inside the reaction tube 2; the sealing sleeve 33 is fixed in the reaction tube 2, wraps the side wall of the feeding tube 31 and can seal the feeding hole 32 of the feeding tube 31; the reset plate 34 is positioned at the upper end of the feed pipe 31 and fixedly connected with the feed pipe 31, and the reset plate 34 is fixedly connected with the lifting rod 22; the first spring 35 is arranged at the bottom of the reset plate 34, and two ends of the first spring are fixedly connected with the upper end of the reaction tube 2 and the lower end of the reset plate 34 respectively; the feed tube 31 can move in and out of the gland 33 as it moves up and down.
In this embodiment, the driving mechanism 4 includes a lifting plate 41, which is located on the top of the tank 1 and is fixedly connected to each lifting rod 22; the supporting frame 42 is arranged at the upper end of the lifting disc 41, and the bottom of the supporting frame extends downwards to pass through the lifting disc 41 to be fixedly connected with the tank body 1; the second spring 43 is arranged at the bottom of the supporting frame 42, and two ends of the second spring are respectively fixedly connected with the bottom of the supporting frame 42 and the top of the lifting disc 41; the motor 44 is arranged at the bottom of the lifting frame; a turntable 45, the center of which is fixedly connected with the output end of the motor 44 and is controlled by the motor 44 to rotate; and a tooth 46 fixed to a side wall of one end of the turntable 45, the tooth 46 being capable of contacting the lifting plate 41 and pressing the lifting plate 41 downward.
In this embodiment, the reaction mechanism 5 includes a reaction kettle 51 for reacting sulfuric acid, ethanol and sodium nitrite; the gas storage tank 52 is communicated with the reaction kettle 51 through a first gas conveying pipe 53, one end of the gas storage tank 52 is provided with a second gas conveying pipe 54, the second gas conveying pipe 54 is provided with a plurality of third gas conveying pipes 55, and each third gas conveying pipe 55 is communicated with one feeding pipe 31; a piston 56 disposed within the air reservoir 52; the electric push rod 57 is arranged on one side of the piston 56 far away from the second air conveying pipe 54, and the electric push rod 57 is arranged on the inner wall of the air storage box 52 and used for controlling the movement of the piston 56; the first air delivery pipe 53 and the second air delivery pipe 54 are both provided with one-way valves.
By the technical scheme, ethanol and sodium nitrite solution are prepared in a reaction kettle, then sulfuric acid is added into the reaction kettle to be mixed with the solution consisting of ethanol and sodium nitrite, ethyl nitrite gas is generated after reaction, ethyl nitrite gas generated in the reaction kettle enters the gas storage tank through the first gas pipe, the check valve on the first gas pipe is closed after the reaction is completed, the gas backflow is avoided, the check valve on the second gas pipe is opened, the piston is pushed by the electric push rod to extrude the ethyl nitrite gas into the feeding pipe, the pressure value in the gas storage box is kept constant all the time (the electric push rod pushes the gas to the right once every time the feeding unit feeds the gas, the pushing distance is the same every time), the gas can enter the reaction pipe with enough power when working, and the gas quantity entering the reaction pipe every time can be guaranteed to be the same through the pressure.
When gas is fed, an electric drive turntable and convex teeth are started to rotate, the turntable drives a gear to rotate downwards to extrude a lifting disc to drive the lifting disc and a lifting rod to move downwards, a reset plate on the lifting rod drives a feed pipe to move downwards to penetrate out of a sealing sleeve, a feed port on the side wall of the feed pipe is not sealed by the sealing sleeve, the feed port is opened, ethyl nitrite gas is added into a reaction pipe, the convex teeth rotate upwards to be not in contact with the lifting disc along with the continuous rotation of the turntable, the reset plates are driven to move upwards to reset from the upper end and the lower end through the elasticity of a first spring and a second spring respectively, the reset plates drive the feed pipe to reset to enter the sealing sleeve again, and the feed port is closed to stop adding the gas; along with the rotation of the motor, the feeding pipe is added with gas once every time the circulating turntable rotates for one circle, and the gas is intermittently added into the reaction pipe to be mixed and reacted with the mixture; carry out the simultaneous input gas from a plurality of points of co-altitude respectively, gas dispersion input, it is even comprehensive with the mixture contact, improve reaction efficiency, realize through the rotation that relies on the motor that intermittent type nature adds gas to the reaction tube, gas addition is stable, convenient, and the packing is added gas after gas mixing reaction is abundant, improves reaction efficiency.
Example 3
As shown in fig. 5 and fig. 6, in this embodiment, the stirring device 6 is further included at the lower end of the feeding pipe 31, and the stirring device 6 includes a mounting bracket 61 fixed on the inner bottom wall of the reaction tube 2; a first rotating shaft 62 horizontally disposed in the reaction tube 2 and rotatably mounted on the mounting frame 61 through a bearing; a helical stirring paddle 63 fixed on the first rotation; a transmission gear 64 fixed on the first rotating shaft 62; and a toothed bar 65 which is vertically arranged in the reaction tube 2 and fixed at the bottom of the feeding tube 31, wherein the toothed bar 65 is in meshing transmission with the transmission gear 64.
In this embodiment, the stirring mechanism 6 further includes a second rotating shaft 66 vertically disposed in the reaction tube 2 and rotatably mounted on the mounting frame 61 through a bearing; a first bevel gear 67 fixed to the first rotating shaft 62; a second bevel gear 68 fixed on the second rotating shaft 66 and in meshed transmission with the first bevel gear 67; and a stirring unit 69 fixed to the second rotating shaft 66.
In this embodiment, the stirring unit 69 includes a stirring plate 691 fixed on the second rotating shaft 66; sliding grooves 692 circumferentially and uniformly provided at the lower end of the agitating plate 691, the width of the sliding grooves 692 gradually decreasing from top to bottom; a slider 693 provided in the slide groove 692 and slidable in the slide groove 692; the stirring rod 694 is vertically arranged at the bottom of the stirring plate 691, one end of the stirring rod 694 extends upwards to penetrate through the sliding groove 692 to be fixedly connected with the sliding block 693, and a balancing weight 695 is fixed at the bottom of the stirring rod 694; the sliding groove 692 is gradually inclined upward from the second rotation shaft 66 to a direction away from the second rotation shaft 66.
According to the technical scheme, when the feeding pipe is controlled by the motor to move up and down, the toothed bar moves up and down along with the feeding pipe, the transmission gear is driven to rotate repeatedly in clockwise and anticlockwise directions, and the first rotating shaft and the spiral stirring paddle are driven to rotate positively and reversely to drive the mixture and the gas to be stirred and mixed; through the rotation of forward and reverse mix, can effectively change the stirring mixing flow direction of mixture, improve mixed reaction efficiency, and need not set up rabbling mechanism specially, receive the coordinated control of motor, control is convenient, just drives the rabbling mechanism stirring when the feeding, and the mixing stirring is timely, can in time mix the gas and the mixture of feeding.
When the first rotating shaft rotates, the first bevel gear rotates along with the first rotating shaft, the second bevel gear and the second rotating shaft are driven to rotate, the stirring disc on the second rotating shaft rotates along with the second rotating shaft, and when the first rotating shaft rotates, the sliding block slides in the sliding groove due to centrifugal force during rotation, namely the sliding block and the stirring rod move towards one end far away from the second rotating shaft, and the mixture is driven to be stirred through stirring of the stirring disc and movement of the stirring rod; when the feeding pipe does not move for feeding, the rotation is stopped, and the sliding block and the stirring rod slide towards the direction close to the rotating shaft under the self gravity and the gravity of the balancing weight; along with repeated feeding, the stirring disc rotates repeatedly, and the puddler removes repeatedly and rotates, and the stirring direction of spiral stirring rake, the stirring direction of rolling disc and the moving direction of puddler all are different, realize mixing the stirring of the multiple angle of mixture and gas when the feeding, increase substantially reaction efficiency.
Example 4
A method for synthesizing materials by using a pipeline reactor is suitable for the pipeline reactor, and in the embodiment of the invention, the method comprises the following steps:
s1: preparing ethanol and sodium nitrite solution in a reaction kettle, adding sulfuric acid into the reaction kettle to mix with the solution consisting of ethanol and sodium nitrite, introducing ethyl nitrite gas generated in the reaction kettle into a gas storage tank through a first gas conveying pipe, closing a one-way valve on the first gas conveying pipe after the reaction is completed, opening a one-way valve on a second gas conveying pipe, pushing a piston through an electric push rod to extrude the ethyl nitrite gas into a feeding pipe, and maintaining the pressure value in the gas storage tank;
s2: adjusting a temperature control device in the tank body, controlling the temperature of a reaction tube to be 18-25 ℃, then preparing a mixture consisting of hydrazine hydrate, sodium hydroxide, a catalyst and ethanol to be input into the reaction tube, and enabling the mixture to spirally flow in the reaction tube and to be fully mixed in the reaction tube through the flip flow of the flip bucket;
s3; starting an electric motor to drive a rotary table and a convex tooth to rotate, wherein the convex tooth rotates downwards to extrude a lifting disc to drive the lifting disc and a lifting rod to move downwards, each feed pipe moves downwards to penetrate out of a sealing sleeve, a feed inlet on each feed pipe is opened to add ethyl nitrite gas into a reaction pipe, reaction pipes with different heights are simultaneously added with equal amounts of ethyl nitrite gas to be mixed with a mixture, the rotary table continues to rotate, the convex tooth rotates upwards until the convex tooth is not contacted with the lifting disc, the lifting rod and the feed pipes are driven to move upwards through the elasticity of a first spring and a second spring, the feed pipes enter the sealing sleeve, the feed inlets are closed to stop adding gas, once gas is added into the feed pipes every time the rotary table rotates one circle along with the rotation of the motor, and the gas is added into the reaction pipes in a clearance manner to be mixed with the mixture;
s4: when the feeding pipe moves up and down, the toothed bar moves up and down along with the feeding pipe, the transmission gear is driven to rotate repeatedly in clockwise and anticlockwise directions, the first rotating shaft and the spiral stirring paddle are driven to rotate forward and turn over to drive a mixture and gas to be stirred and mixed, the first bevel gear rotates along with the first rotating shaft and drives the second bevel gear and the second rotating shaft to rotate, the stirring disc rotates along with the first rotating shaft, the sliding block and the stirring bar move towards one end far away from the second rotating shaft during rotation to drive the mixture to be stirred, after rotation is stopped, the sliding block and the stirring bar move towards the direction close to the rotating shaft, and the stirring bar moves repeatedly and rotates to stir and mix the mixture and the gas repeatedly in a stirring direction different from that of the spiral stirring paddle;
s5: and (3) reacting the mixture and gas in a reaction tube for 1-2 hours, introducing all the gas in the first half hour, then distilling the finally obtained reaction liquid under reduced pressure to recover ethanol, carrying out suction filtration to obtain a wet product, and then drying under reduced pressure to obtain a fixed product.
Wherein the catalyst is tributylamine; when the sulfuric acid is added, the temperature of a solution consisting of ethanol and sodium nitrite is kept at 0-5 ℃, and the molar ratio of the added sulfuric acid to the ethanol to the sodium nitrite is 1: 2.17: 2.04, the added sulfuric acid is a sulfuric acid solution with the mass concentration of 20-40%; the sulfuric acid solution is continuously added at the speed of 10-20g/min, and the molar ratio of the introduced ethyl nitrite gas to the hydrazine hydrate, the sodium hydroxide, the catalyst and the ethanol is 1: 1-1.2: 0.5-1: 0.03-0.05: 2-3; and (3) removing entrained acid from the ethyl nitrite by water washing, and then introducing into a mixture of hydrazine hydrate, sodium hydroxide, a catalyst and ethanol.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A pipeline reactor, characterized by: comprises that
The temperature control device is arranged in the tank body, and the heat transfer layer is arranged outside the tank body;
the reaction tube is spirally wound outside the tank body;
the dosing mechanism comprises a plurality of dosing units which are uniformly arranged around the circumferential direction of the tank body at intervals;
the driving mechanism is used for controlling the dosing mechanism to simultaneously add gas materials into the reaction tubes at different heights outside the tank body in an interval mode;
the reaction mechanism is used for reacting sulfuric acid, ethanol and sodium nitrite and storing the produced ethyl nitrite gas;
and a flip bucket is arranged on the inner wall of the reaction tube.
2. A pipeline reactor according to claim 1, wherein: the medicine adding unit comprises
The lifting rod is vertically arranged outside the induction pipe and is controlled by the driving mechanism to lift;
the feeding units are uniformly arranged at one end of the lifting rod close to the dosing mechanism, and the feeding units are arranged at different heights and respectively feed materials corresponding to the reaction tubes at one height; each feeding unit is communicated with the reaction mechanism.
3. A pipeline reactor according to claim 2, wherein: the feed unit comprises
The feeding pipe is vertically arranged at the upper end of the reaction pipe, the lower end of the feeding pipe is inserted into the reaction pipe, and a feeding hole is formed in part of the side wall of the feeding pipe, which is positioned in the reaction pipe;
the sealing sleeve is fixed in the reaction tube, wraps the side wall of the feeding tube and can seal the feeding hole of the feeding tube;
the reset plate is positioned at the upper end of the feeding pipe and fixedly connected with the feeding pipe, and the reset plate is fixedly connected with the lifting rod;
the first spring is arranged at the bottom of the reset plate, and two ends of the first spring are respectively and fixedly connected with the upper end of the reaction tube and the lower end of the reset plate;
the feed pipe can pass in and out the sealing sleeve when moving up and down.
4. A pipeline reactor according to claim 2, wherein: the driving mechanism comprises
The lifting disc is positioned at the top of the tank body and is fixedly connected with each lifting rod;
the supporting frame is arranged at the upper end of the lifting disc, and the bottom of the supporting frame extends downwards to pass through the lifting disc to be fixedly connected with the tank body;
the second spring is arranged at the bottom of the support frame, and two ends of the second spring are respectively fixedly connected with the bottom of the support frame and the top of the lifting disc;
the motor is arranged at the bottom of the lifting frame;
the center of the turntable is fixedly connected with the output end of the motor and is controlled by the motor to rotate;
and the convex teeth are fixed on the side wall at one end of the rotary disc and can be in contact with the lifting disc and can extrude and move the lifting disc downwards.
5. A pipeline reactor according to claim 3, wherein: the reaction mechanism comprises
The reaction kettle is used for the reaction of sulfuric acid, ethanol and sodium nitrite;
the gas storage tank is communicated with the reaction kettle through a first gas pipe, a second gas pipe is arranged at one end of the gas storage tank, a plurality of third gas pipes are arranged on the second gas pipe, and each third gas pipe is communicated with one feeding pipe;
the piston is arranged in the air storage box;
the electric push rod is arranged on one side of the piston, which is far away from the second gas transmission pipe, and the electric push rod is arranged on the inner wall of the gas storage box and used for controlling the movement of the piston;
and the first air conveying pipe and the second air conveying pipe are respectively provided with a one-way valve.
6. A pipe reactor according to claim 3 or 4 or 5, wherein: still including locating the rabbling mechanism of inlet pipe lower extreme, the rabbling mechanism includes
The mounting frame is fixed on the inner bottom wall of the reaction tube;
the first rotating shaft is horizontally arranged in the reaction tube and is rotatably arranged on the mounting frame through a bearing;
the spiral stirring paddle is fixed on the first rotation;
the transmission gear is fixed on the first rotating shaft;
and the toothed bar is vertically arranged in the reaction tube and fixed at the bottom of the feeding tube, and the toothed bar is in meshing transmission with the transmission gear.
7. A pipeline reactor according to claim 6, wherein: the stirring mechanism further comprises
The second rotating shaft is vertically arranged in the reaction tube and is rotatably arranged on the mounting frame through a bearing;
the first conical gear is fixed on the first rotating shaft;
the second bevel gear is fixed on the second rotating shaft and is in meshing transmission with the first bevel gear;
and the stirring unit is fixed on the second rotating shaft.
8. A pipeline reactor according to claim 7, wherein: the stirring unit comprises
The stirring disc is fixed on the second rotating shaft;
the sliding grooves are circumferentially and uniformly formed in the lower end of the stirring plate, and the width of each sliding groove is gradually reduced from top to bottom;
the sliding block is arranged in the sliding groove and can slide in the sliding groove;
the stirring rod is vertically arranged at the bottom of the stirring disc, one end of the stirring rod extends upwards to penetrate through the sliding groove to be fixedly connected with the sliding block, and a balancing weight is fixed at the bottom of the stirring rod;
the sliding groove gradually inclines upwards from the second rotating shaft to the direction far away from the second rotating shaft.
9. A method for synthesizing materials by using a pipeline reactor is suitable for the pipeline reactor and is characterized by comprising the following steps:
s1: preparing ethanol and sodium nitrite solution in a reaction kettle, adding sulfuric acid into the reaction kettle to mix with the solution consisting of ethanol and sodium nitrite, introducing ethyl nitrite gas generated in the reaction kettle into a gas storage tank through a first gas conveying pipe, closing a one-way valve on the first gas conveying pipe after the reaction is completed, opening a one-way valve on a second gas conveying pipe, pushing a piston through an electric push rod to extrude the ethyl nitrite gas into a feeding pipe, and maintaining the pressure value in the gas storage tank;
s2: adjusting a temperature control device in the tank body, controlling the temperature of a reaction tube to be 18-25 ℃, then preparing a mixture consisting of hydrazine hydrate, sodium hydroxide, a catalyst and ethanol to be input into the reaction tube, and enabling the mixture to spirally flow in the reaction tube and to be fully mixed in the reaction tube through the flip flow of the flip bucket;
s3; starting an electric motor to drive a rotary table and a convex tooth to rotate, wherein the convex tooth rotates downwards to extrude a lifting disc to drive the lifting disc and a lifting rod to move downwards, each feed pipe moves downwards to penetrate out of a sealing sleeve, a feed inlet on each feed pipe is opened to add ethyl nitrite gas into a reaction pipe, reaction pipes with different heights are simultaneously added with equal amounts of ethyl nitrite gas to be mixed with a mixture, the rotary table continues to rotate, the convex tooth rotates upwards until the convex tooth is not contacted with the lifting disc, the lifting rod and the feed pipes are driven to move upwards through the elasticity of a first spring and a second spring, the feed pipes enter the sealing sleeve, the feed inlets are closed to stop adding gas, once gas is added into the feed pipes every time the rotary table rotates one circle along with the rotation of the motor, and the gas is added into the reaction pipes in a clearance manner to be mixed with the mixture;
s4: when the feeding pipe moves up and down, the toothed bar moves up and down along with the feeding pipe, the transmission gear is driven to rotate repeatedly in clockwise and anticlockwise directions, the first rotating shaft and the spiral stirring paddle are driven to rotate forward and turn over to drive a mixture and gas to be stirred and mixed, the first bevel gear rotates along with the first rotating shaft and drives the second bevel gear and the second rotating shaft to rotate, the stirring disc rotates along with the first rotating shaft, the sliding block and the stirring bar move towards one end far away from the second rotating shaft during rotation to drive the mixture to be stirred, after rotation is stopped, the sliding block and the stirring bar move towards the direction close to the rotating shaft, and the stirring bar moves repeatedly and rotates to stir and mix the mixture and the gas repeatedly in a stirring direction different from that of the spiral stirring paddle;
s5: and (3) reacting the mixture and gas in a reaction tube for 1-2 hours, introducing all the gas in the first half hour, then distilling the finally obtained reaction liquid under reduced pressure to recover ethanol, carrying out suction filtration to obtain a wet product, and then drying under reduced pressure to obtain a fixed product.
10. A pipeline reactor according to claim 9, wherein: the catalyst in step S2 is tributylamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210600064.XA CN114797739B (en) | 2022-05-27 | 2022-05-27 | Pipeline reactor and method for synthesizing materials by using same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210600064.XA CN114797739B (en) | 2022-05-27 | 2022-05-27 | Pipeline reactor and method for synthesizing materials by using same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114797739A true CN114797739A (en) | 2022-07-29 |
| CN114797739B CN114797739B (en) | 2023-10-13 |
Family
ID=82518286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210600064.XA Active CN114797739B (en) | 2022-05-27 | 2022-05-27 | Pipeline reactor and method for synthesizing materials by using same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114797739B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150202590A1 (en) * | 2012-07-24 | 2015-07-23 | Evonik Industries Ag | Process for preparing alkenylhalosilanes and reactor suitable therefor |
| CN105600912A (en) * | 2016-03-10 | 2016-05-25 | 西安交通大学 | Multi-point oxygen injection and subsection mixing device for supercritical water oxidizing reaction tubular reactor |
| CN111250028A (en) * | 2020-03-26 | 2020-06-09 | 河南城建学院 | Maillard reactor for recycling rectifying tower bottoms in soybean processing |
| CN111437791A (en) * | 2020-05-12 | 2020-07-24 | 合肥福纳科技有限公司 | Reactor and reaction system for quantum dot synthesis |
| WO2022068057A1 (en) * | 2020-09-30 | 2022-04-07 | 广东石油化工学院 | Continuous production method for 2,4-dinitrochlorobenzene |
| CN216457017U (en) * | 2021-12-20 | 2022-05-10 | 青岛科技大学 | Radial flow spiral tube type crystallizer |
-
2022
- 2022-05-27 CN CN202210600064.XA patent/CN114797739B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150202590A1 (en) * | 2012-07-24 | 2015-07-23 | Evonik Industries Ag | Process for preparing alkenylhalosilanes and reactor suitable therefor |
| CN105600912A (en) * | 2016-03-10 | 2016-05-25 | 西安交通大学 | Multi-point oxygen injection and subsection mixing device for supercritical water oxidizing reaction tubular reactor |
| CN111250028A (en) * | 2020-03-26 | 2020-06-09 | 河南城建学院 | Maillard reactor for recycling rectifying tower bottoms in soybean processing |
| CN111437791A (en) * | 2020-05-12 | 2020-07-24 | 合肥福纳科技有限公司 | Reactor and reaction system for quantum dot synthesis |
| WO2022068057A1 (en) * | 2020-09-30 | 2022-04-07 | 广东石油化工学院 | Continuous production method for 2,4-dinitrochlorobenzene |
| CN216457017U (en) * | 2021-12-20 | 2022-05-10 | 青岛科技大学 | Radial flow spiral tube type crystallizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114797739B (en) | 2023-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN116196832B (en) | Cleanup additive preparation device with anti-deposition function for oil field | |
| CN114797739A (en) | Pipeline reactor and method for synthesizing materials by using same | |
| CN111686628A (en) | Quick lime agitated vessel of energy cyclic utilization | |
| CN207980976U (en) | A kind of lubricating oil mixing plant | |
| CN216778815U (en) | Production equipment of nano metal copper oxide | |
| CN218222411U (en) | High-efficient reation kettle of hydrogen fluoride | |
| CN112811393B (en) | Diborane preparation device and diborane preparation method | |
| CN213254463U (en) | Metal working fluid stirred tank | |
| CN205222706U (en) | System for continuous production hangs down impurity magnesium silicide | |
| CN114146612A (en) | Automatic cuprous chloride feeding process | |
| CN106672980A (en) | Reactor with spiral conveying and method for continuous production of magnesium silicide with low impurity | |
| CN206843083U (en) | A kind of new reacting furnace for preparing potassium sulfate | |
| CN213854590U (en) | Improved mercury-free catalyst soaking tank | |
| CN217910413U (en) | Gas stirring device with function of preventing admixture from precipitating | |
| CN212284034U (en) | A high-efficient synthesizer for synthesizing lithium hexafluorophosphate | |
| CN219559630U (en) | Airtight reation kettle is used in aprepitant production | |
| CN216063076U (en) | Stirring equipment for production and processing of solid-state lithium ion battery material | |
| CN218590506U (en) | Reaction equipment for producing organic carbonate | |
| CN117339536B (en) | Stirring equipment and method for high-temperature materials | |
| CN215611250U (en) | Glass reactor for medicine preparation suitable for polytetrafluoroethylene treatment | |
| CN212576284U (en) | Heating device for aerosol spray production | |
| CN216259196U (en) | High-efficient reation kettle is used in ammonium chloride purification | |
| CN218688794U (en) | Energy-saving speed-regulating stirring equipment for liquid detergent | |
| CN218554082U (en) | Chemical reaction kettle | |
| CN215183266U (en) | Manufacturing equipment of spherical silver powder for solar front silver paste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |