Separation equipment for preparing low free isocyanate polyurethane prepolymer
By designing a separation device for the preparation of low-free isocyanate polyurethane prepolymers, the problems of free diisocyanate monomers and solid impurities in the polyurethane prepolymers are solved, and efficient material separation and simplified process flow are achieved.
Patent Information
- Application Number
- CN202311347619.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-18
- Publication Date
- 2025-04-18
AI Technical Summary
During the preparation of polyurethane prepolymer, a certain amount of free diisocyanate monomer is present, resulting in a complex preparation process, large investment, and solid impurities, affecting the later distillation treatment.
A separation device for the preparation of low-free isocyanate polyurethane prepolymers is designed, including separation reactors, stirring columns, lifting channels, rotating shafts, stirring structures, water bath heating components and vacuum pumps. Through circumferential and longitudinal stirring, scraping treatment and circulating filtration, combined with water bath heating and vacuum negative pressure, the efficient separation of materials is achieved.
Through the use of this separation equipment, the stirring effect is significantly improved, the impurity content is reduced, the later distillation treatment is simplified, and the complexity and investment cost of the equipment are reduced.
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Figure CN119838537A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical equipment, in particular to separation equipment for preparing low-free isocyanate polyurethane prepolymer. Background Art
[0002] When preparing polyurethane prepolymers, a stoichiometric excess of diisocyanate (MDI / TDI, etc.) and polyol (polyester / polyether, etc.) are usually mixed and reacted to form an isocyanate-terminated prepolymer. In the polyurethane prepolymer prepared by this method, there will inevitably be a certain amount of free diisocyanate monomers, generally reaching about 1-10%. These residual monomers will cause several adverse effects. The method of vacuum decompression distillation can reduce the degree and time of chemical reactions, and the obtained prepolymer is purer without other impurities remaining. However, the overall equipment process is more complicated and the investment is large. In order to reduce the content of residual monomers, other solid impurities will also be generated during the preparation process, which is not conducive to the subsequent distillation treatment. During the separation process, the raw materials need to be fully mixed and stirred, otherwise it will cause local reactions on the inner wall of the reactor, resulting in the problem of increased impurity content. It is also necessary to remove impurities that cannot react in time to ensure the quality of the reaction.
[0003] Based on this, a separation device for preparing a low-free isocyanate polyurethane prepolymer is now provided, which can eliminate the disadvantages of the existing devices. Summary of the invention
[0004] The object of the present invention is to provide a separation device for preparing a low-free isocyanate polyurethane prepolymer to solve the problems in the background technology.
[0005] To achieve the above object, the present invention provides the following technical solutions: The separation equipment for preparing low-free isocyanate polyurethane prepolymer comprises a separation reaction kettle and a plurality of legs arranged at the lower end thereof, wherein the upper end of the separation reaction kettle is provided with a feeding port for feeding, the upper end of the feeding port is provided with a movable door, the middle bottom of the separation reaction kettle is provided with a discharge pipe for discharging, the lower end of the discharge pipe is connected to a solid-liquid separator for further separation, the outer side of the separation reaction kettle is provided with a water bath heating component for heating, the uniformity of heating can be ensured by the water bath heating component, the upper end of the separation reaction kettle is provided with a condensation box, and the discharge end of the condensation box is provided with a liquid for storing cold water. A storage box for condensed material, a stirring column is provided in the middle position of the separation reactor, a lifting channel is provided at the lower end of the stirring column, a rotating shaft is coaxially provided inside the lifting channel, a lifting blade for pushing the liquid upward is provided on the outer side of the rotating shaft, the stirring column and the rotating shaft are connected to a driving component for driving the rotation thereof, a stirring structure for stirring is provided at the lower end of the rotating shaft, a vacuum pump for extracting the air inside the separation reactor is provided at the upper end of the separation reactor, at least one overflow pipe is provided on the outer side of the upper end of the stirring column, and a filtering component for filtering the material is provided on the inner wall of the separation reactor.
[0006] On the basis of the above technical solution, the present invention also provides the following optional technical solution: In an optional scheme: the filtering component includes an aggregate ring arranged inside the separation reactor, the aggregate ring is rotatably connected to the inner wall of the separation reactor, the aggregate ring is fixedly connected to the stirring column through a filter connecting rod, the outer end of the overflow pipe is projected into the aggregate ring, a filter plate for filtering materials is provided at the bottom of the aggregate ring, and a cleaning component for cleaning the bottom surface of the aggregate cone is provided on the right side of the separation reactor.
[0007] In an optional scheme: the cleaning component includes a horizontal transverse tube arranged on the right side of the separation reactor, the left end of the horizontal transverse tube is in contact with the bottom of the filter plate, the upper end surface of the filter plate is matched with a cleaning plate, the cleaning plate is connected and fixed to the top of the separation reactor through a suspension rod, a piston block is matched in the horizontal transverse tube, the right end of the piston block is connected to the left end of the pull rod, the right end of the pull rod is connected to the output end of the horizontal push rod, and a discharge vertical pipe for discharging is provided on the lower right side of the horizontal transverse tube.
[0008] In an optional scheme: the stirring structure includes a mounting frame arranged at the lower end of the rotating shaft, a stirring shaft is rotatably provided at the end of the mounting frame, a plurality of floating springs are distributed on the outside of the stirring shaft, a friction wheel is slidably provided at the lower end of the mounting frame, an aggregate cone bottom is provided at the bottom of the separation reactor, the friction wheel is in friction contact with the inner wall of the aggregate cone bottom, a limiting ring for limiting the friction wheel is provided on the inner wall of the aggregate cone bottom, the friction wheel and the stirring shaft are connected by a rotating limiting piece, a plurality of stirring rods are distributed on the outside of the stirring shaft, a scraper cross bar is provided on the outer side of the upper end of the stirring column, a scraper plate is provided at the end of the scraper cross bar, and the scraper plate is in contact with the inner wall of the separation reactor.
[0009] In an optional solution: the rotation limiting member includes a limiting groove arranged on the outer side of the stirring shaft, and the inner wall of the friction wheel is provided with a limiting protrusion matching with the limiting groove.
[0010] In an optional scheme: the driving component includes a second friction disk arranged at the upper end of the rotating shaft, a first friction disk is provided at the upper end of the stirring column, an intermediate friction wheel is provided between the second friction disk and the first friction disk, the intermediate friction wheel is connected to a driving motor for driving it to rotate, a plurality of contraction rods are provided at the lower end of the driving motor, a contraction sleeve is slidably provided at the lower end of the contraction rod, a contraction spring for connecting the contraction rod is provided inside the contraction sleeve, the lower end of the contraction sleeve is connected to the upper end of the separation reactor, and the intermediate friction wheel is an elliptical structure, which can make the second friction disk rise and fall, thereby making the stirring structure float up and down.
[0011] In an optional solution: the second friction disk is connected to the first friction disk via a reset member, the reset member includes a floating spring, and the second friction disk and the first friction disk are rotated relative to each other and provided with a rotating ring connected to the floating spring.
[0012] In an optional solution: the water bath heating component includes a water bath heating jacket arranged outside the separation reactor, a heat insulation layer is distributed outside the water bath heating jacket, and an electric heating tube is arranged inside the water bath heating jacket.
[0013] Compared with the prior art, the present invention has the following beneficial effects: The present invention is designed to address the deficiencies of the prior art. While stirring the material circumferentially, it can also stir it longitudinally by floating up and down, and at the same time, scrape the inner wall of the separation reactor. In addition, it can also achieve circulating filtration of the material, which greatly improves the stirring effect so that impurities can be removed smoothly in the later stage. In addition, the stirring here is combined with water bath heating and vacuum negative pressure to smoothly discharge impurities, and it is highly practical. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 It is a structural schematic diagram of the present invention.
[0015] Figure 2 It is a structural schematic diagram of the lower side of the present invention.
[0016] Figure 3 It is a schematic diagram of the internal structure of the present invention.
[0017] Figure 4 It is a partial enlarged view of the structure of the present invention.
[0018] Notes on figure numbers: separation reactor 11, water bath heating jacket 12, discharge vertical pipe 13, horizontal cross pipe 14, horizontal push rod 15, piston block 16, hole cleaning plate 17, suspension rod 18, contraction spring 19, contraction rod 21, contraction sleeve 20, drive motor 22, intermediate friction wheel 23, first friction disc 24, floating spring 25, second friction disc 26, stirring column 27, lifting channel 28, lifting blade 29, overflow pipe 31, condensation box 30, filter connecting rod 32, aggregate ring 33, filter plate 34, stirring rod 35, stirring shaft 36, limit ring 37, friction wheel 38, mounting frame 39, discharge pipe 40, solid-liquid separator 41, support leg 42, aggregate cone bottom 43, scraper plate 44. DETAILED DESCRIPTION
[0019] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments.
[0020] In one embodiment, Figure 1-Figure 4As shown, a separation device for preparing a low-free isocyanate polyurethane prepolymer comprises a separation reactor 11 and a plurality of legs 42 arranged at the lower end thereof, wherein a feeding port for feeding is arranged at the upper end of the separation reactor 11, a discharge pipe 40 for discharging is arranged at the middle bottom of the separation reactor 11, and the lower end of the discharge pipe 40 is connected to a solid-liquid separator 41 for further separation, a water bath heating component for heating is arranged on the outer side of the separation reactor 11, and the uniformity of heating can be ensured by the water bath heating component, a condensation box 30 is arranged at the discharge port position at the upper end of the separation reactor 11, and a storage box for storing condensed material is arranged at the discharge end of the condensation box 30, and a stirring device is arranged at the middle position of the separation reactor 11. A column 27, a lifting channel 28 is provided at the lower end of the stirring column 27, a rotating shaft is coaxially provided inside the lifting channel 28, a lifting blade 29 is provided on the outer side of the rotating shaft for pushing the liquid upward, the stirring column 27 and the rotating shaft are connected to a driving component for driving the rotating shaft, a stirring structure for stirring is provided at the lower end of the rotating shaft, a vacuum pump for extracting the air inside the separation reactor 11 is provided at the upper end of the separation reactor 11, thereby reducing the boiling point of the distillation, at least one overflow pipe 31 is provided on the outer side of the upper end of the stirring column 27, and a filtering component for filtering the material is provided on the inner wall of the separation reactor 11, so that the solid impurities in the material can be removed to prevent the impurities from staying and affecting the reaction; The filtering component includes a collection ring 33 arranged inside the separation reaction kettle 11, the collection ring 33 is rotatably connected to the inner wall of the separation reaction kettle 11, the collection ring 33 is fixedly connected to the stirring column 27 through a filter connecting rod 32, the outer end of the overflow pipe 31 is projected into the collection ring 33, and a filter plate 34 for filtering materials is provided at the bottom of the collection ring 33. A cleaning component for cleaning the surface of the collection cone bottom 43 is provided on the right side of the separation reaction kettle 11. The cleaning component can maintain the filtering effect of the filter plate 34 to avoid clogging problems; The cleaning assembly includes a horizontal transverse tube 14 arranged on the right side of the separation reactor 11, the left end of the horizontal transverse tube 14 contacts the bottom of the filter plate 34, the upper end surface of the filter plate 34 is matched with a cleaning plate 17, the cleaning plate 17 is connected and fixed to the top of the separation reactor 11 through a suspension rod 18, and a piston block 16 is matched in the horizontal transverse tube 14, the right end of the piston block 16 is connected to the left end of the pull rod, and the right end of the pull rod is connected to the output end of the horizontal push rod 15, and a discharge vertical pipe 13 for discharging is provided on the lower right side of the horizontal transverse tube 14, so that when discharging in the later stage, it is only necessary to drive the piston block 16 to move to the right through the horizontal push rod 15, so that impurities can be extracted from the position of the cleaning plate 17, thereby completing the slag discharge process; The stirring structure includes a mounting frame 39 arranged at the lower end of the rotating shaft, a stirring shaft 36 is rotatably arranged at the end of the mounting frame 39, a plurality of floating springs 25 are distributed on the outer side of the stirring shaft 36, a friction wheel 38 is slidably arranged at the lower end of the mounting frame 39, a collection cone bottom 43 is arranged at the bottom of the separation reactor 11, the friction wheel 38 is in friction contact with the inner wall of the collection cone bottom 43, a limiting ring 37 is arranged on the inner wall of the collection cone bottom 43 to limit the friction wheel 38, and a rotating limiting member is provided between the friction wheel 38 and the stirring shaft 36 The stirring shaft 36 is connected to the stirring column 27, and a plurality of stirring rods 35 are distributed on the outside of the stirring shaft 36. When the mounting frame 39 rotates with the rotating shaft, the friction between the friction wheel 38 and the aggregate cone bottom 43 drives the stirring shaft 36 to rotate, thereby driving the stirring rod 35 to rotate and stir the material. A scraping cross bar is provided on the outside of the upper end of the stirring column 27, and a scraping plate 44 is provided at the end of the scraping cross bar. The scraping plate 44 is in contact with the inner wall of the separation reaction kettle 11, so that the inner wall of the separation reaction kettle 11 can be scraped while stirring, thereby ensuring the mixing effect. The rotation limiting member includes a limiting groove arranged on the outside of the stirring shaft 36, and the inner wall of the friction wheel 38 is provided with a limiting protrusion matched with the limiting groove, so that the friction wheel 38 and the stirring shaft 36 cannot rotate relative to each other, but can slide relative to each other; The driving component includes a second friction disk 26 arranged at the upper end of the rotating shaft, a first friction disk 24 is arranged at the upper end of the stirring column 27, an intermediate friction wheel 23 is arranged between the second friction disk 26 and the first friction disk 24, the intermediate friction wheel 23 is connected to a driving motor 22 for driving the intermediate friction wheel 23 to rotate, a plurality of contraction rods 21 are arranged at the lower end of the driving motor 22, a contraction sleeve 20 is slidably arranged at the lower end of the contraction rod 21, a contraction spring 19 for connecting the contraction rod 21 is arranged inside the contraction sleeve 20, and the lower end of the contraction sleeve 20 is connected to the upper end of the separation reactor 11. It should be noted that the intermediate friction wheel 23 here is an elliptical structure, which can make the second friction disk 26 fluctuate up and down, so that the stirring structure floats up and down, thereby improving the stirring effect; The second friction disc 26 is connected to the first friction disc 24 via a reset member, and the reset member includes a floating spring 25. The second friction disc 26 and the first friction disc 24 rotate relative to each other and are provided with a rotating ring connected to the floating spring 25, so that the second friction disc 26 can press the middle friction wheel 23 tightly. The water bath heating component includes a water bath heating jacket 12 arranged on the outside of the separation reactor 11, an insulation layer is distributed on the outside of the water bath heating jacket 12, an electric heating tube is arranged inside the water bath heating jacket 12, and a temperature sensor for detecting the heating temperature is arranged inside the water bath heating jacket 12, so that the temperature of the water bath heating can be controlled.
[0021] The above-mentioned embodiment discloses a separation device for preparing a low-free isocyanate polyurethane prepolymer, wherein, in actual use, the material is fed into the separation reactor 11 along the feed port, the separation reactor 11 is placed in a vacuum state by a vacuum pump, and then the inner wall of the separation reactor 11 is heated by a water bath heating component. While heating, the stirring column 27 and the rotating shaft are driven to rotate by a driving component. The stirring rod 35 and the stirring shaft 36 can also float up and down when stirring the material circumferentially, and the scraping of the scraper plate 44 is combined to eliminate the stirring dead angle and prevent impurities from staying in a local position. During stirring, the material will be fed into the collecting ring 33 to filter the material. After filtering, the cleaning plate 17 will remove the impurities at the horizontal cross tube 14 position, and then cooperate with the piston block 16 to slide outward to complete the discharge process.
[0022] The above is only a specific implementation of the present disclosure, but the protection scope of the present disclosure is not limited thereto. Any person skilled in the art who is familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present disclosure, which should be included in the protection scope of the present disclosure. Therefore, the protection scope of the present disclosure should be based on the protection scope of the claims.
Claims
1. A separation device for preparing a low-free isocyanate polyurethane prepolymer, comprising a separation reaction kettle (11) and a plurality of legs (42) arranged at the lower end thereof, wherein the upper end of the separation reaction kettle (11) is provided with a feeding port for feeding, and the upper end of the feeding port is provided with a movable door, and the middle bottom of the separation reaction kettle (11) is provided with a discharge pipe (40) for discharging materials, and the lower end of the discharge pipe (40) is connected to a solid-liquid separator (41) for further separation, and the outer side of the separation reaction kettle (11) is provided with a water bath heating component for heating; It is characterized in that A condensation box (30) is provided at the discharge port position at the upper end of the separation reaction kettle (11), and a storage box for storing condensed material is provided at the discharge end of the condensation box (30). A stirring column (27) is provided in the middle position of the separation reaction kettle (11), and a lifting channel (28) is provided at the lower end of the stirring column (27). A rotating shaft is coaxially provided inside the lifting channel (28), and a lifting blade (29) for pushing liquid upward is provided on the outer side of the rotating shaft. The stirring column (27) and the rotating shaft are connected to a driving component for driving the rotating shaft to rotate, and a stirring structure for stirring is provided at the lower end of the rotating shaft. A vacuum pump for extracting air from the separation reaction kettle (11) is provided at the upper end of the separation reaction kettle (11), and at least one overflow pipe (31) is provided on the outer side of the upper end of the stirring column (27). A filtering component for filtering materials is provided on the inner wall of the separation reaction kettle (11).
2. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 1, characterized in that The filtering component comprises a material collecting ring (33) arranged inside the separation reaction kettle (11); the material collecting ring (33) is rotatably connected to the inner wall of the separation reaction kettle (11); the material collecting ring (33) is fixedly connected to the stirring column (27) via a filtering connecting rod (32); the outer end of the overflow pipe (31) is projected into the material collecting ring (33); a filtering plate (34) for filtering materials is provided at the bottom of the material collecting ring (33); and a cleaning component for cleaning the surface of the material collecting cone bottom (43) is provided on the right side of the separation reaction kettle (11).
3. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 2, characterized in that: The cleaning assembly comprises a horizontal transverse tube (14) arranged on the right side of the separation reactor (11), the left end of the horizontal transverse tube (14) contacts the bottom of the filter plate (34), the upper end surface of the filter plate (34) is provided with a cleaning plate (17), the cleaning plate (17) is connected and fixed to the top of the separation reactor (11) through a suspension rod (18), a piston block (16) is provided in the horizontal transverse tube (14), the right end of the piston block (16) is connected to the left end of the pull rod, the right end of the pull rod is connected to the output end of the horizontal push rod (15), and a discharge vertical pipe (13) for discharging is provided on the lower right side of the horizontal transverse tube (14).
4. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 1, characterized in that The stirring structure comprises a mounting frame (39) arranged at the lower end of the rotating shaft, a stirring shaft (36) is rotatably provided at the end of the mounting frame (39), a plurality of floating springs (25) are distributed on the outer side of the stirring shaft (36), a friction wheel (38) is slidably provided at the lower end of the mounting frame (39), a collection cone bottom (43) is provided at the inner bottom of the separation reaction kettle (11), the friction wheel (38) is in frictional contact with the inner wall of the collection cone bottom (43), a limiting ring (37) for limiting the friction wheel (38) is provided on the inner wall of the collection cone bottom (43), the friction wheel (38) and the stirring shaft (36) are connected via a rotating limiting member, a plurality of stirring rods (35) are distributed on the outer side of the stirring shaft (36), a scraping cross bar is provided on the outer side of the upper end of the stirring column (27), a scraping plate (44) is provided at the end of the scraping cross bar, and the scraping plate (44) is in contact with the inner wall of the separation reaction kettle (11).
5. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 4, characterized in that The rotation limiting member comprises a limiting groove arranged on the outside of the stirring shaft (36), and the inner wall of the friction wheel (38) is provided with a limiting protrusion matching the limiting groove.
6. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 1, characterized in that: The driving component comprises a second friction disk (26) arranged at the upper end of the rotating shaft, a first friction disk (24) is arranged at the upper end of the stirring column (27), an intermediate friction wheel (23) is arranged between the second friction disk (26) and the first friction disk (24), the intermediate friction wheel (23) is connected to a driving motor (22) for driving the intermediate friction wheel (23) to rotate, a plurality of contraction rods (21) are arranged at the lower end of the driving motor (22), a contraction sleeve (20) is slidably arranged at the lower end of the contraction rod (21), a contraction spring (19) for connecting the contraction rod (21) is arranged inside the contraction sleeve (20), the lower end of the contraction sleeve (20) is connected to the upper end of the separation reaction kettle (11), the intermediate friction wheel (23) is an elliptical structure, the elliptical structure can make the second friction disk (26) rise and fall, thereby making the stirring structure float up and down, and the second friction disk (26) and the first friction disk (24) are connected by a reset member.
7. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymers according to claim 6, characterized in that The reset element comprises a floating spring (25), and the second friction disc (26) and the first friction disc (24) are provided with a rotating ring connected to the floating spring (25) for rotation relative to each other.
8. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 1, characterized in that: The water bath heating component comprises a water bath heating jacket (12) arranged outside the separation reaction kettle (11), a heat insulation layer is distributed outside the water bath heating jacket (12), and an electric heating pipe is arranged inside the water bath heating jacket (12).
9. The separation device for preparing storage-stable low-free isocyanate polyurethane prepolymer according to claim 6, characterized in that: The intermediate friction wheel (23), the second friction plate (26) and the first friction plate (24) are replaced with gears that mesh with each other.