CN114436989A - Preparation process and device of bisoxazoline - Google Patents

Preparation process and device of bisoxazoline Download PDF

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Publication number
CN114436989A
CN114436989A CN202111605165.8A CN202111605165A CN114436989A CN 114436989 A CN114436989 A CN 114436989A CN 202111605165 A CN202111605165 A CN 202111605165A CN 114436989 A CN114436989 A CN 114436989A
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CN
China
Prior art keywords
reaction kettle
bisoxazoline
fixedly connected
catalyst
central tube
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Pending
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CN202111605165.8A
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Chinese (zh)
Inventor
蒙健
仲维龙
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Jiangsu Weunite Fine Chemical Co ltd
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Jiangsu Weunite Fine Chemical Co ltd
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Priority to CN202111605165.8A priority Critical patent/CN114436989A/en
Publication of CN114436989A publication Critical patent/CN114436989A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D263/00—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings
    • C07D263/02—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings not condensed with other rings
    • C07D263/08—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
    • C07D263/10—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to ring carbon atoms
    • C07D263/12—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to ring carbon atoms with radicals containing only hydrogen and carbon atoms
    • 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
    • B01J19/18—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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • 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
    • B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
    • 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
    • B01J4/008—Feed or outlet control devices
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/002—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor with a moving instrument
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/082—Controlling processes
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087—Heating or cooling 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135—Electric resistance heaters

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention relates to the field of preparation of bisoxazoline, in particular to a preparation process and a device of the bisoxazoline, and the process comprises the following steps: s1, adding carboxylic acid and alkanolamine into the reaction kettle; s2, starting a stirring mechanism in the reaction kettle and a heating mechanism, and filling a catalyst into the reaction kettle at a constant speed to obtain the bisoxazoline; and S3, performing discharging operation. The invention has better mixing effect, improves the mixing speed and the mixing uniformity of the catalyst and the reactants, improves the integral reaction speed, replaces the traditional stirring assembly and reduces the reaction time.

Description

Preparation process and device of bisoxazoline
Technical Field
The invention relates to the field of preparation of bisoxazoline, in particular to a process and a device for preparing bisoxazoline.
Background
Tradition is carrying out the bisoxazoline preparation in-process, through in throwing into reation kettle with the raw materials, under stirring and heating condition, add the catalyst and react, traditional stirring and material addition mode are through directly throwing into reation kettle with the catalyst, start rabbling mechanism, the stirring subassembly mixes the stirring to reactant and catalyst, the stirring in-process, the distribution diffusion velocity of catalyst is slow, the catalyst is not abundant with the reactant contact of each department, cause reaction rate slow, cause the stirring time long, the productivity is unsatisfactory.
Disclosure of Invention
Based on the defects in the prior art mentioned in the background art, the invention provides a preparation process and a device of the bisoxazoline.
The invention overcomes the technical problems by adopting the following technical scheme, and specifically comprises the following steps:
a preparation process of bisoxazoline comprises the following steps:
s1, adding carboxylic acid and alkanolamine into the reaction kettle;
s2, starting a stirring mechanism in the reaction kettle and a heating mechanism, and filling a catalyst into the reaction kettle at a constant speed to obtain the bisoxazoline;
and S3, performing discharging operation.
Preferably, the heating mechanism keeps the reaction temperature in the reaction kettle at 100-200 ℃.
Preferably, the carboxylic acid is terephthalic acid or isophthalic acid.
Preferably, the alkanolamine is ethanolamine or isopropanolamine.
Preferably, the catalyst is hypophosphorous acid or alkyl hypophosphorous acid.
A bisoxazoline production apparatus comprising:
the reaction kettle is vertically arranged on the base;
the reaction kettle comprises a central cylinder which is arranged in the reaction kettle and fixedly connected with a reaction kettle bottom plate and is provided with openings at the upper end and the lower end, and a material pressing disc which is sleeved outside the central cylinder and is in sliding butt joint with the inner wall of the reaction kettle; and a central tube mounted in the central tube and having an upper end extending above the reaction vessel;
the material pressing disc is connected with a lifting mechanism for driving the material pressing disc to move up and down in the reaction kettle, the upper end of the central tube is communicated with a catalyst feeding mechanism arranged on a top plate of the reaction kettle, and the central tube is positioned in the central cylinder and is internally provided with spray holes which are distributed at equal intervals;
catalyst feeding mechanism includes the inlet pipe that passes through the rotary joint intercommunication with the center tube upper end, with inlet pipe intercommunication and fixed mounting the material pump on the reation kettle roof, through pipeline and material pump intercommunication and install the catalyst section of thick bamboo on the reation kettle roof.
Preferably, the lifting mechanism comprises a group of vertical rods fixedly connected with the upper end face of the material pressing disc and penetrating through the top plate of the reaction kettle, connecting rods fixedly connected with the upper ends of the vertical rods and in an inverted L shape, moving blocks fixedly connected with the connecting rods, chute plates provided with the moving blocks for sliding up and down and fixedly connected with the side walls of the reaction kettle, lead screws installed in the chute plates and in threaded connection with the moving blocks, transmission shafts connected with the lower ends of the lead screws through a first transmission gear set, rotary drums connected with the transmission shafts through a second transmission gear set, discharge pipes communicated with the lower ends of the reaction kettle and embedded in the inner sides of the rotary drums, worm wheels fixedly sleeved with the rotary drums, worms meshed with the worm wheels and horizontally arranged, and a first motor fixedly connected with the worms through a coupler and fixedly connected with the base.
Preferably, the central tube is fixedly connected with an upper stirring blade at a position above the central tube, and the upper end of the central tube is connected with the screw rod for transmission through a transmission belt.
Preferably, a heating device is installed in the shell of the central cylinder, and the heating device is heating wires distributed spirally.
Preferably, the upper end of the reaction kettle is communicated with a feeding pipe; the discharging mechanism comprises a discharging pipe, a movable plunger, a threaded rod, a prism shaft and a second motor, wherein the discharging pipe is communicated with the discharging pipe and is obliquely arranged, the movable plunger is arranged at the communicating position of the discharging pipe and the reaction kettle, the upper end of the movable plunger is fixedly connected with the lower end of the movable plunger, the threaded rod is in threaded connection with a bottom plate of the discharging pipe, the prism shaft is embedded in the threaded rod in a spline embedding mode, and the second motor is connected with the prism shaft through a coupler and is fixedly connected with the base.
After adopting the structure, compared with the prior art, the invention has the following advantages:
the invention has the advantages that the central cylinder, the central pipe which is provided with the spray hole and is communicated with the catalyst feeding mechanism and the pressure plate which is nested in the reaction kettle and is sleeved outside the central cylinder are arranged in the central cylinder, in the reaction process, the lifting mechanism drives the pressure plate to move up and down, the pressure plate presses the reactant in the reaction kettle into the central cylinder to be fully contacted with the catalyst sprayed into the central cylinder, the invention has better mixing effect, improves the mixing speed and the mixing uniformity of the catalyst and the reactant, improves the integral reaction speed, replaces the traditional stirring assembly, and reduces the reaction time.
The discharging device comprises a movable plunger, a lower stirring blade, a discharging pipe which is communicated with the discharging pipe and is obliquely arranged, a threaded rod which is arranged at the bottom of the movable plunger, and a prism shaft which is arranged in the threaded rod in a spline nesting mode, so that discharging is convenient, and during discharging, the movable plunger and the lower stirring blade which move up and down are utilized to improve discharging speed.
Drawings
Fig. 1 is a schematic perspective view of the front side view of a bisoxazoline production apparatus.
Fig. 2 is a schematic perspective view of a back view of a bisoxazoline production apparatus.
Fig. 3 is a schematic view of the internal cross-sectional structure in the reaction vessel in the bisoxazoline production apparatus.
Fig. 4 is a schematic sectional view of the internal structure in the center cylinder of the bisoxazoline production apparatus.
Fig. 5 is a schematic perspective view of a central tube in the bisoxazoline manufacturing apparatus.
Fig. 6 is a schematic view showing an assembly structure of a threaded rod and a prism shaft in the bisoxazoline manufacturing apparatus.
In the figure: 1. a reaction kettle; 2. pressing a material plate; 3. a vertical rod; 4. a connecting rod; 5. a moving block; 6. a chute plate; 7. a screw rod; 8. a first drive gear set; 9. a drive shaft; 10. a second drive gear set; 11. a rotating drum; 12. a worm gear; 13. a worm; 14. a first motor; 15. a central barrel; 16. heating wires; 17. a central tube; 18. spraying a hole; 19. a rotary joint; 20. a feed pipe; 21. a material pumping pump; 22. a catalyst cartridge; 23. a feeding pipe; 24. a discharge pipe; 25. a discharge pipe; 26. an upper stirring blade; 27. a lower stirring blade; 28. moving the plunger; 29. a threaded rod; 30. a prismatic shaft; 31. a second motor; 32. a transmission belt; 33. a base.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Referring to fig. 1 to 6, in an embodiment of the present invention, a process for preparing a bisoxazoline includes the following steps:
s1, adding carboxylic acid and alkanolamine into the reaction kettle;
s2, starting a stirring mechanism in the reaction kettle and a heating mechanism, and filling a catalyst into the reaction kettle at a constant speed to obtain the bisoxazoline;
and S3, performing discharging operation.
Wherein, the heating mechanism keeps the reaction temperature in the reaction kettle at 100-200 ℃.
Wherein the carboxylic acid is terephthalic acid or isophthalic acid.
Wherein the alkanolamine is ethanolamine or isopropanolamine.
Wherein the catalyst is hypophosphorous acid or alkyl hypophosphorous acid.
In particular, the preparation of the bisoxazoline is carried out by the process, the process is simple, and the reaction conditions are easy to control.
A bisoxazoline production apparatus comprising:
a base 33 and a reaction kettle 1 vertically installed on the base 33;
the device comprises a central cylinder 15 which is arranged in a reaction kettle 1 and fixedly connected with a bottom plate of the reaction kettle 1 and is provided with openings at the upper end and the lower end, and a material pressing plate 2 which is sleeved outside the central cylinder 15 and is in sliding butt joint with the inner wall of the reaction kettle 1; and a central tube 17 installed in the central tube 15 and having an upper end extending above the reaction tank 1;
the pressure material tray 2 is connected with a lifting mechanism for driving the pressure material tray 2 to move up and down in the reaction kettle 1, the upper end of the central tube 17 is communicated with a catalyst feeding mechanism arranged on the top plate of the reaction kettle 1, and the part of the central tube 17, which is positioned in the central cylinder 15, is provided with spray holes 18 which are distributed at equal intervals;
the catalyst feeding mechanism comprises a feeding pipe 20 communicated with the upper end of the central pipe 17 through a rotary joint 19, a pumping pump 21 communicated with the feeding pipe 20 and fixedly installed on the top plate of the reaction kettle 1, and a catalyst cylinder 22 communicated with the pumping pump 21 through a pipeline and installed on the top plate of the reaction kettle 1.
Specifically, elevating system drives pressure flitch 2 and reciprocates in the ring chamber between a central section of thick bamboo 15 and reation kettle 1 inner wall, impresses the opening at the upper and lower both ends of a central section of thick bamboo 15 with the reactant in the ring chamber in a central section of thick bamboo 15, simultaneously, catalyst feed mechanism carries out the efficient with the reactant that flows in a central section of thick bamboo 15 in injecting a central section of thick bamboo 15 with the catalyst through center tube 17 and mixes for the high-efficient even diffusion of catalyst is in the reactant, improves the compounding effect, reaction rate with higher speed.
In this embodiment, the central cylinder 15 is a hollow cylinder, and the lower end of the central cylinder 15 is fixedly connected to the bottom plate of the reaction kettle 1 through a support rod.
In another embodiment of the invention, the lifting mechanism comprises a group of vertical rods 3 which are fixedly connected with the upper end surface of the material pressing plate 2 and penetrate through the top plate of the reaction kettle 1, connecting rods 4 which are fixedly connected with the upper ends of the vertical rods 3 and are in an inverted L shape, the reaction kettle comprises a moving block 5 fixedly connected with a connecting rod 4, a chute plate 6 which is provided for the moving block 5 to slide up and down and is fixedly connected with the side wall of the reaction kettle 1, a screw rod 7 which is installed in the chute plate 6 and is in threaded connection with the moving block 5, a transmission shaft 9 which is connected with the lower end of the screw rod 7 through a first transmission gear set 8, a rotary drum 11 which is connected with the transmission shaft 9 through a second transmission gear set 10, a discharge pipe 24 which is communicated with the lower end of the reaction kettle 1 and is embedded in the inner side of the rotary drum 11, a worm wheel 12 which is fixedly sleeved with the rotary drum 11, a worm 13 which is meshed with the worm wheel 12 and is horizontally arranged, and a first motor 14 which is connected with the worm 13 through a coupler and is fixedly connected with a base 33.
Specifically, first motor 14 drives rotary drum 11 through worm 13 and worm wheel 12 and rotates, rotary drum 11 drives the transmission shaft 9 rotation of both sides through second drive gear group 10, transmission shaft 9 drives lead screw 7 and rotates, lead screw 7 drives movable block 5 and removes in chute board 6, movable block 5 drives pressure charging tray 2 through connecting rod 4 and vertical pole 3 and removes, it needs to explain that, first motor 14 is just reversing motor, and then realize reciprocating of pressure charging tray 2, make the even mixture through a center section of thick bamboo 15 and catalyst efficient of material.
In another embodiment of the present invention, the lifting mechanism is a hydraulic cylinder fixedly connected to the pressure plate 2.
In another embodiment of the invention, the central tube 17 is fixedly connected with an upper stirring blade 26 at a position above the central tube 15, and the upper end of the central tube 17 is connected with the screw rod 7 for transmission through a transmission belt 32.
Specifically, the screw rod 7 extends to the upper part of the chute plate 6 and drives the central pipe 17 to rotate by a transmission belt 32, and the central pipe 17 drives the upper stirring blade 26 to rotate, so that the material moving to the upper outlet of the central cylinder 15 is centrifugally diffused by the upper stirring blade 26, and the diffusion speed of the catalyst and the reactant is accelerated.
In another embodiment of the present invention, a heating device is installed in the housing of the central cylinder 15, and the heating device is a heating wire 16 distributed in a spiral shape.
Specifically, the heating wire 16 is connected to an external power supply, wherein it should be noted that the central cylinder 15 is made of a heat conducting material, so that heat generated by the heating wire 16 is diffused to the central cylinder 15, and the flow of reactants in the central cylinder 15 accelerates heat exchange, improves heating effect, ensures reaction temperature, and improves heating efficiency.
In another embodiment of the invention, the upper end of the reaction kettle 1 is communicated with a feeding pipe 23; the lower end of the reaction kettle 1 is provided with a discharging mechanism, the discharging mechanism comprises a discharging pipe 25 which is communicated with a discharging pipe 24 and is obliquely arranged, a movable plunger 28 which is arranged at the communication position of the discharging pipe 24 and the reaction kettle 1 and is fixedly connected with a lower stirring blade 27 at the upper end, a threaded rod 29 which is fixedly connected with the lower end of the movable plunger 28 and is in threaded connection with a bottom plate of the discharging pipe 24, a prismatic shaft 30 which is embedded in the threaded rod 29 in a spline embedding mode, and a second motor 31 which is connected with the prismatic shaft 30 through a coupler and is fixedly connected with a base 33.
Specifically, the second motor 31 drives the prism shaft 30 to rotate, the prism shaft 30 drives the threaded rod 29 to rotate, under the effect of the threaded hole of the discharge pipe 24, the threaded rod 29 drives the movable plunger 28 to rotate up and down in the discharge pipe 24, the material enters the discharge pipe 25 through the discharge pipe 24 to be discharged, and under the centrifugal pushing of the lower stirring blade 27, the material is conveniently discharged, and the material is prevented from remaining in the discharge pipe 24.
In this embodiment, the discharge pipe 24 is a cylinder with an open upper end, and the bottom plate of the discharge pipe 24 is provided with a threaded hole matched with the threaded rod 29; the threaded rod 29 is provided with a prism cavity matched with the prism shaft 28, and the prism shaft 28 is nested in the prism cavity and is in sliding connection with the inner wall of the prism cavity.
The working principle is as follows:
the first motor 14 drives the rotating drum 11 to rotate through the worm 13 and the worm wheel 12, the rotating drum 11 drives the transmission shafts 9 on two sides to rotate through the second transmission gear set 10, the transmission shafts 9 drive the lead screws 7 to rotate, the lead screws 7 drive the moving block 5 to move in the chute plates 6, and the moving block 5 drives the material pressing discs 2 to move through the connecting rods 4 and the vertical rods 3. it should be noted that the first motor 14 is a forward and reverse rotating motor, so that the material pressing discs 2 can move up and down, and meanwhile, the material can be uniformly mixed with the catalyst efficiently through the central cylinder 15, and the catalyst feeding mechanism injects the catalyst into the central cylinder 15 through the central pipe 17 to be efficiently mixed with the reactant flowing in the central cylinder 15;
meanwhile, the heating wire 16 is connected with an external power supply, wherein it should be noted that the central cylinder 15 is made of a heat conducting material, so that heat generated by the heating wire 16 is diffused to the central cylinder 15, and reactants flow in the central cylinder 15, thereby accelerating heat exchange, improving heating effect and ensuring reaction temperature;
during the ejection of compact, prismatic axle 30 is driven to rotate by second motor 31, and prismatic axle 30 drives threaded rod 29 and rotates, and under the screw hole effect of discharging pipe 24, threaded rod 29 drives and moves plunger 28 and rotate about in discharging pipe 24, and the material enters into row material pipe 25 through discharging pipe 24 and discharges, under the centrifugation of stirring leaf 27 down promotes, conveniently carries out the ejection of compact.
The foregoing is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. But all changes which come within the scope of the invention are intended to be embraced therein.

Claims (10)

1. A preparation process of bisoxazoline is characterized by comprising the following steps:
s1, adding carboxylic acid and alkanolamine into the reaction kettle;
s2, starting a stirring mechanism in the reaction kettle and a heating mechanism, and filling a catalyst into the reaction kettle at a constant speed to obtain the bisoxazoline;
and S3, performing discharging operation.
2. The process according to claim 1, wherein the heating means is used to maintain the reaction temperature in the reaction vessel at 100-200 ℃.
3. The process according to claim 1, wherein the carboxylic acid is terephthalic acid or isophthalic acid.
4. The process according to claim 1, wherein the alkanolamine is ethanolamine or isopropanolamine.
5. The process according to claim 1, wherein the catalyst is hypophosphorous acid or alkyl hypophosphorous acid.
6. A bisoxazoline production apparatus, comprising:
a base (33) and a reaction kettle (1) vertically arranged on the base (33);
the device comprises a central cylinder (15) which is arranged in a reaction kettle (1) and fixedly connected with a bottom plate of the reaction kettle (1) and is provided with openings at the upper end and the lower end, and a material pressing disc (2) which is sleeved on the outer side of the central cylinder (15) and is in sliding butt joint with the inner wall of the reaction kettle (1); and a central tube (17) which is arranged in the central tube (15) and the upper end of which extends to the upper part of the reaction kettle (1);
the pressure feed tray (2) is connected with a lifting mechanism for driving the pressure feed tray (2) to move up and down in the reaction kettle (1), the upper end of the central tube (17) is communicated with a catalyst feeding mechanism arranged on a top plate of the reaction kettle (1), and the central tube (17) is positioned in the central tube (15) and is internally provided with spray holes (18) which are distributed at equal intervals;
the catalyst feeding mechanism comprises a feeding pipe (20) communicated with the upper end of the central pipe (17) through a rotary joint (19), a pumping pump (21) communicated with the feeding pipe (20) and fixedly installed on the top plate of the reaction kettle (1), and a catalyst cylinder (22) communicated with the pumping pump (21) through a pipeline and installed on the top plate of the reaction kettle (1).
7. The device for preparing the bisoxazoline according to claim 6, wherein the lifting mechanism comprises a group of vertical rods (3) which are fixedly connected with the upper end surface of the material pressing disc (2) and penetrate through the top plate of the reaction kettle (1), a connecting rod (4) which is fixedly connected with the upper end of the vertical rods (3) and is in an inverted L shape, a moving block (5) which is fixedly connected with the connecting rod (4), a chute plate (6) which is provided for the moving block (5) to slide up and down and is fixedly connected with the side wall of the reaction kettle (1), a screw rod (7) which is arranged in the chute plate (6) and is in threaded connection with the moving block (5), a transmission shaft (9) which is connected with the lower end of the screw rod (7) through a first transmission gear group (8), a rotary drum (11) which is connected with the transmission shaft (9) through a second transmission gear group (10), and a discharge pipe (24) which is communicated with the lower end of the reaction kettle (1) and is embedded in the inner side of the rotary drum (11), The worm gear (12) is fixedly sleeved with the rotary drum (11), the worm (13) is meshed with the worm gear (12) and horizontally arranged, and the first motor (14) is connected with the worm (13) through a coupler and is fixedly connected with the base (33).
8. The bisoxazoline preparation apparatus according to claim 7, wherein the central tube (17) is fixedly connected with an upper stirring blade (26) at a position above the central tube (15), and the upper end of the central tube (17) is connected with the screw rod (7) for transmission through a transmission belt (32).
9. The apparatus for preparing bisoxazoline according to claim 7, wherein a heating means is installed in the housing of the central cylinder (15), and the heating means is a heating wire (16) which is spirally distributed.
10. The apparatus for preparing bisoxazoline according to claim 7, wherein a feeding pipe (23) is connected to the upper end of the reaction vessel (1); reation kettle (1) lower extreme is equipped with discharge mechanism, discharge mechanism includes row material pipe (25) that set up with discharging pipe (24) intercommunication and slope, install removal plunger (28) of stirring leaf (27) under discharging pipe (24) and reation kettle (1) intercommunication department and upper end fixedly connected with, threaded rod (29) with removal plunger (28) lower extreme fixed connection and with discharging pipe (24) bottom plate threaded connection, prism axle (30) through nested mode nestification of spline in threaded rod (29), be connected through shaft coupling and prism axle (30) and with base (33) fixed connection's second motor (31).
CN202111605165.8A 2021-12-24 2021-12-24 Preparation process and device of bisoxazoline Pending CN114436989A (en)

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Application Number Priority Date Filing Date Title
CN202111605165.8A CN114436989A (en) 2021-12-24 2021-12-24 Preparation process and device of bisoxazoline

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Application Number Priority Date Filing Date Title
CN202111605165.8A CN114436989A (en) 2021-12-24 2021-12-24 Preparation process and device of bisoxazoline

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CN114436989A true CN114436989A (en) 2022-05-06

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CN117380121A (en) * 2023-09-25 2024-01-12 安徽尖峰北卡药业有限公司 Production process and safe production system of lenvatinib mesylate

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117380121A (en) * 2023-09-25 2024-01-12 安徽尖峰北卡药业有限公司 Production process and safe production system of lenvatinib mesylate
CN117380121B (en) * 2023-09-25 2024-05-14 安徽尖峰北卡药业有限公司 Production process and safe production system of lenvatinib mesylate

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