Device for continuously producing polyether ester

Abstract

The invention provides a device for continuously producing polyether ester, and relates to the field of polyether ester synthesis. The continuous polyether ester production device comprises a dissolver, an esterification reactor, a neutralization reactor, a storage tank, a condenser and a plate-and-frame filter press, raw materials pass through the dissolver, the esterification reactor, the neutralization reactor, the esterification reactor and the plate-and-frame filter press to generate products, the products are stored in the storage tank, and the condenser is used for discharging water in the esterification reactor and the neutralization reactor. The esterification reactor comprises a tank body, a stirring assembly, a water vapor discharging assembly, a feeding assembly and a discharging assembly. According to the device for continuous production of polyether ester, a high-pressure nitrogen environment can be achieved, the reaction effect is better, the efficiency is higher through the arrangement of the negative-pressure exhaust pipe, the nitrogen pressing-in pipe and the nitrogen replenisher, water molecules can be condensed during continuous exhaust through the arrangement of the water vapor discharging assembly, the water removal effect is better, and during water removal, the continuous production of polyether ester is achieved. The reaction process is constant in pressure and is still in a nitrogen protection environment.

Description

Technical Field

[0001] The present invention relates to the field of polyether ester synthesis, and particularly to a device for continuous production of polyether ester. Background Art

[0002] Polyether ester (Polyether Ester) is a class of copolymers composed of polyether and polyester blocks, combining the flexibility of polyether and the strength and chemical resistance of polyester. The following are its main characteristics and applications: Characteristics Flexibility: The polyether segment provides good elasticity. Strength: The polyester segment imparts high mechanical strength. Chemical resistance: Good tolerance to a variety of chemicals. Thermal stability: Stable performance at high temperatures. Processability: Easy to process by injection molding, extrusion, etc. Applications Elastomers: Used to manufacture high-elasticity materials. Fibers: Used to produce high-performance fibers. Films: Used for packaging and industrial films. Engineering plastics: Used for components in the fields of automobiles, electronics, etc. Adhesives and coatings: Used for high-performance adhesives and coatings. Common types Polyether ester elastomer (TPEE): Has rubber elasticity and plastic strength. Polyether ester block copolymer: Combines the excellent properties of polyether and polyester. Advantages Comprehensive performance: Combines flexibility and strength. Chemical resistance: Suitable for a variety of chemical environments. Thermal stability: Suitable for high-temperature applications.

[0003] The esterification reaction of polyether ester is a key step in the preparation of polyether ester copolymers. Through the esterification reaction of polyether and polyester prepolymers, polymer chains are formed. The detailed process of the esterification reaction is as follows:

[0004] 1. Raw material preparation, polyether diol, catalyst, additives: such as antioxidants, stabilizers, etc. 2. Prepolymerization reaction mixture. 3. Removal of by-products and dehydration. 4. Further polymerization and temperature increase. 5. Termination of reaction and cooling. Discharging: Taking out the product from the reaction kettle. 6. Post-treatment and granulation. Key control points Raw material ratio: Precise control of the ratio of polyether diol and dibasic acid. Reaction temperature: Strict control of the temperature at each stage. Catalyst dosage: Appropriate amount of catalyst to control the reaction rate. Dehydration: Effective removal of water to improve the reaction efficiency. Reaction mechanism The esterification reaction mainly includes the following steps: Esterification: The polyether diol reacts with the dibasic acid to form an ester bond and water. Polycondensation: The prepolymer further undergoes polycondensation to form polymer chains and release water.

[0005] However, the current esterification reactor cannot achieve a completely vacuum effect in an environment with nitrogen protection, and pressure or decompression is required during nitrogen protection. As a result, the generated water vapor cannot be completely discharged, so subsequent dehydration of the raw materials is still required. Moreover, multiple pipelines are provided at the bottom of the existing reaction kettle, with a complex structure. When the reaction rate is slow during the reaction of the raw materials, some materials will accumulate in the equipment gaps and are difficult to participate in the reaction. Summary of the Invention

[0006] In view of the deficiencies of the prior art, the present invention provides a device for continuous production of polyether ester, which solves the problems raised in the above background art.

[0007] To achieve the above objectives, the present invention is realized through the following technical solutions: A device for continuous production of polyether ester includes a dissolver, an esterification reactor, a neutralization reactor, a storage tank, a condenser, and a plate and frame filter press. The raw materials pass through the dissolver, esterification reactor, neutralization reactor, esterification reactor, and plate and frame filter press to generate products into the storage tank. The condenser is used to discharge the water contained in the esterification reactor and the neutralization reactor. The esterification reactor includes a tank body, a stirring assembly, a water vapor discharge assembly, a feeding assembly, and a discharging assembly. A plurality of nitrogen replenishers are installed at the bottom of the tank body. A negative pressure suction pipe and a nitrogen pressure inlet pipe are respectively installed on one side of the top of the tank body. The outer ring of the tank body is covered with a one-way heater for heating the tank body;

[0008] The water vapor discharge assembly is installed inside the tank body. The water vapor discharge assembly includes a spiral pipe and a joint. The joint penetrates the tank body and the one-way heater. The spiral pipe is arranged inside the tank body and is coaxially arranged with the tank body. The spiral pipe is connected and communicated with the joint;

[0009] The feeding assembly is installed on one side of the upper end of the tank body. The feeding assembly includes a feeding pipe, a hydraulic cylinder A, a connecting shaft, and a piston. The feeding pipe is installed at the upper end of the tank body and is communicated with its interior. There are two pistons, both fixedly connected to the connecting shaft. The pistons slide sealingly on the inner wall of the feeding pipe. The hydraulic cylinder A is fixed to the outer wall of the feeding pipe. The output shaft of the hydraulic cylinder A is fixed to the end of the connecting shaft outside the feeding pipe.

[0010] Preferably, the stirring assembly includes a motor, a transmission shaft, a connecting rod, a paddle, and an impeller. The motor is fixed at the top end of the tank body. The transmission shaft is connected to the output shaft of the motor. The other end of the transmission shaft is inserted into the tank body. The transmission shaft is rotationally connected to the top end of the tank body in a sealed manner. The bottom end of the tank body is of a hemispherical structure. The connecting rod is fixed to the bottom end of the transmission shaft. The connecting rod is fixedly connected to the paddle through a reinforcement device. The impeller is fixed to the connecting rod.

[0011] Preferably, the discharging assembly includes a discharging pipe, a hydraulic cylinder B, a connector, a sealing ring, a concentric sleeve, and a discharge pipe. The discharging pipe is fixedly installed at the center position of the bottom of the tank body. The discharging pipe is communicated with the interior of the tank body. The top end of the discharging pipe extends into the interior of the tank body and is flush with the inner bottom wall of the tank body. The hydraulic cylinder B is inserted into the bottom end of the discharging pipe. The connector fixedly connects the two. The sealing ring seals the outer wall of the hydraulic cylinder B and the inner wall of the discharging pipe. A sealing plug is fixedly installed on the output shaft of the hydraulic cylinder B. The outer ring of the sealing plug slides sealingly on the inner wall of the discharging pipe;

[0012] A plurality of discharge holes are provided on the side wall of the blanking pipe. The concentric sleeve is fixedly sleeved outside the blanking pipe. The discharge holes communicate with the inside of the concentric sleeve. The discharge pipe is fixed to and communicates with one side of the concentric sleeve. When the sealing plug moves to the lowermost position, it is below the discharge holes.

[0013] Preferably, the nitrogen replenisher is located at the bottom end of the tank body. There are three nitrogen replenishers. One end of them connected to the tank body extends into the interior of the bottom end of the tank body and fits the arc surface of the inner wall of the bottom end of the tank body.

[0014] Preferably, the top surface of the sealing plug is an arc-shaped groove structure. When the sealing plug extends to the uppermost end, it is flush with the inner wall of the lower end of the tank body, forming a complete spherical surface.

[0015] Preferably, the spiral pipe is wound around the transmission shaft. The spiral pipe is located in the middle of the tank body and is suspended. The spiral pipe is divided into an outer spiral part and an inner spiral part. The inner spiral part is inside the outer spiral part, and there is an equidistant gap between the two. One ends of the outer spiral part and the inner spiral part away from the tank body (1) are both fixed to the joint. The inner spiral part is connected to the condenser and the vacuum unit through the joint for cooling the inner spiral part and pumping air.

[0016] Preferably, the upper end of the tank body is a hemispherical structure. The negative pressure extraction pipe and the nitrogen pressure injection pipe are both installed on this hemispherical structure.

[0017] Preferably, the flap is an arc-shaped structure. The outer shape of the flap is the same as the outer shape of the bottom of the tank body, and the bottom end of the flap fits the inner wall of the bottom of the tank body.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. For the device for continuous production of polyether ester, by setting the negative pressure extraction pipe, the nitrogen pressure injection pipe and the nitrogen replenisher, during the prepolymerization reaction, polyether diol and dibasic acid are mixed in proportion, and air is extracted outward through the negative pressure extraction pipe. At this time, multiple nitrogen replenishers will replenish nitrogen into the interior of the tank body from the bottom. After a period of circulation, the interior of the tank body is basically completely filled with nitrogen. At this time, the state of carrying out the reaction by heating is carried out under complete nitrogen protection. If pressurization is required, nitrogen is further injected through the nitrogen pressure injection pipe. Before that, the interior of the tank body should be completely filled with nitrogen. Therefore, a high-pressure nitrogen environment can be achieved, and the reaction effect is better and the efficiency is higher.

[0020] 2. The device for continuous production of polyether ester, by setting up a steam discharge component, after reacting for a period of time, the internal pressure of the tank can be reduced by pumping air outwards through the suction pipe. After the pressure reduction, water molecules condense into vapor. At this time, the spiral pipe continuously pumps air outwards, and the nitrogen gas inlet pipe cooperates with it to further supplement dry nitrogen gas into the tank to keep the pressure in the tank constant. When the spiral pipe continuously pumps air outwards, the gas circulates along the spiral pipe. The other end of the spiral pipe is connected to a condenser, so the temperature gradually decreases along the pipe body. Therefore, water molecules can be condensed during continuous air extraction, and the water removal effect is good. Moreover, during water removal, the reaction process is under constant pressure and still in an environment protected by nitrogen gas.

[0021] 3. The device for continuous production of polyether ester, by setting up a feeding component, when adding the esterifying agent, the connecting shaft is pulled out by the hydraulic cylinder A, and the esterifying agent is placed between the two pistons. When the connecting shaft is pressed in, the two pistons cooperate with the feeding pipe to seal the esterifying agent. As one piston enters the interior of the tank, the esterifying agent will automatically fall into the tank. Therefore, when adding, only a very small amount of external gas enters the tank. With the cooperation of the nitrogen gas replenisher and the negative pressure suction pipe, the mixed external gas can be removed as soon as possible.

[0022] 4. The device for continuous production of polyether ester, by setting up a stirring component, the stirring component is concentrated below the tank to accelerate the mixing of raw materials.

[0023] 5. The device for continuous production of polyether ester, by setting up a feeding and discharging component, the hydraulic cylinder B can maintain a high-pressure sealing state before feeding and discharging. In addition, the sealing plug can maintain the integrity of the inner wall of the tank, which is convenient for the mixing of raw materials and avoids the accumulation of raw materials at the gaps, affecting the progress of the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the production process of the present invention;

[0025] Figure 2 It is a structural diagram of the esterification reactor of the present invention;

[0026] Figure 3 It is a structural diagram of the bottom of the tank of the present invention;

[0027] Figure 4 It is a structural diagram of the interior of the tank of the present invention;

[0028] Figure 5 For the present invention Figure 4 The enlarged structural diagram at position A;

[0029] Figure 6 It is a structural diagram of the steam discharge component of the present invention;

[0030] Figure 7 For the present inventionFigure 6 Enlarged view of the structure at position B in the middle;

[0031] Figure 8 Schematic diagram of the bottom structure of the tank body of the present invention;

[0032] Figure 9 Schematic diagram of the structure of the blanking assembly of the present invention;

[0033] Figure 10 Schematic diagram of the structure of the spiral tube of the present invention;

[0034] Figure 11 Distribution diagram of the internal air flow of the tank body of the present invention.

[0035] In the figure: 1. Tank body; 2. Stirring assembly;

[0036] 201. Motor; 202. Transmission shaft; 203. Connecting rod; 204. Paddle; 205. Impeller; 206. Reinforcer;

[0037] 3. Steam discharge assembly;

[0038] 301. Spiral tube;

[0039] 3011. Outer spiral part; 3012. Inner spiral part;

[0040] 302. Joint;

[0041] 4. Feeding assembly;

[0042] 401. Feeding pipe; 402. Hydraulic cylinder A; 403. Connecting shaft; 404. Piston;

[0043] 5. Blanking assembly;

[0044] 501. Blanking pipe; 502. Hydraulic cylinder B; 503. Connector; 504. Sealing ring; 505. Concentric sleeve; 506. Discharge pipe; 507. Sealing plug; 508. Discharge hole;

[0045] 6. Nitrogen replenisher; 7. Negative pressure suction pipe; 8. Nitrogen pressure inlet pipe; 9. One-way heater. Detailed implementation manners

[0046] Next, the technical solutions in the embodiments of the present application will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the scope of protection of the present application.

[0047] It should be noted that all the directional indications in the embodiments of the present application are only used to explain the relative positional relationship and movement conditions between components in a specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0048] In the present application, unless otherwise clearly defined and limited, the terms "connection", "fixation", etc. shall be understood in a broad sense. For example, "fixation" can be a fixed connection, a detachable connection, or an integral body; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal communication of two components or the interaction relationship between two components, unless otherwise clearly limited. For those of ordinary skill in the art, the specific meanings of the above terms in the present application can be understood according to specific circumstances.

[0049] In addition, in the present application, the descriptions such as "first", "second", etc. are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions between various embodiments can be combined with each other, but it must be based on the ability of those of ordinary skill in the art to implement. When the combination of technical solutions results in contradictions or cannot be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by the present application.

[0050] As Figures 1 - 11 shown, a device for continuous production of polyether ester includes a dissolver, an esterification reactor, a neutralization reactor, a storage tank, a condenser, and a plate and frame filter press. The raw materials pass through the dissolver, the esterification reactor, the neutralization reactor, the esterification reactor, and the plate and frame filter press to generate products into the storage tank. The condenser is used to discharge the water contained in the esterification reactor and the neutralization reactor. The esterification reactor includes a tank body 1, a stirring assembly 2, a water vapor discharge assembly 3, a feeding assembly 4, and a discharging assembly 5. A plurality of nitrogen replenishers 6 are installed at the bottom of the tank body 1. A negative pressure suction pipe 7 and a nitrogen pressure inlet pipe 8 are respectively installed on one side of the top of the tank body 1. The outer ring of the tank body 1 is covered with a one-way heater 9 for heating the tank body 1;

[0051] The water vapor discharge assembly 3 is installed inside the tank body 1. The water vapor discharge assembly 3 includes a spiral pipe 301 and a joint 302. The joint 302 penetrates through the tank body 1 and the one-way heater 9. The spiral pipe 301 is arranged inside the tank body 1 and is coaxially arranged with the tank body 1. The spiral pipe 301 is connected and communicated with the joint 302;

[0052] The feeding assembly 4 is installed on one side of the upper end of the tank body 1. The feeding assembly 4 includes a feeding pipe 401, a hydraulic cylinder A402, a connecting shaft 403 and a piston 404. The feeding pipe 401 is installed on the upper end of the tank body 1 and is connected to the interior thereof. Two pistons 404 are provided, both of which are fixed on the connecting shaft 403. The piston 404 slides in a sealed manner with the inner wall of the feeding pipe 401. The hydraulic cylinder A402 is fixed to the outer wall of the feeding pipe 401. The output shaft of the hydraulic cylinder A402 is fixed to one end of the connecting shaft 403 outside the feeding pipe 401.

[0053] The raw materials first pass through the dissolver, then come to the esterification reactor for esterification reaction, and then enter the neutralization reactor, and finally pass through the plate and frame filter press and are stored in the storage tank. The bottom of the tank body 1 of the esterification reactor is equipped with legs, the nitrogen supplementer 6 is connected to the nitrogen tank or nitrogen pump, and the negative pressure exhaust pipe 7 needs to be connected to the vacuum pump component. The nitrogen pressure inlet pipe 8 is connected to the same position as the nitrogen supplementer 6, but both have electromagnetic valves that can be opened and closed remotely. All solenoid valves are connected to the central processing component for control of the intelligent terminal. The one-way heater 9 is also controlled by the intelligent chip. A temperature sensor is provided inside it for real-time monitoring of temperature changes to create a suitable reaction temperature in the tank body 1.

[0054] The outer end of the joint 302 is connected to the condenser and the vacuum unit to achieve negative pressure extraction, and the condenser can reduce the temperature of the spiral tube 301 when cooling down. The spiral tube 301 adopts a copper tube, which has good heat transfer performance. When water molecules condense, they can be gathered and collected by the spiral tube 301. When exhausting, the water vapor will slowly gather into large water droplets in the spiral tube 301, which can achieve a high efficiency of water vapor extraction, and the extracted water resources can be reused in the later stage.

[0055] The outer ring of the piston 404 is provided with a piston ring made of rubber material, so an interference fit relationship is adopted between the piston 404 and the feeding pipe 401. A large pressure is required to press the piston 404 into the feeding pipe 401. Therefore, a hydraulic cylinder A402 is adopted. The hydraulic cylinder A402 can achieve better sealing, and when the temperature and pressure inside the tank body 1 are high, leakage is unlikely to occur.

[0056] The stirring assembly 2 includes a motor 201, a transmission shaft 202, a connecting rod 203, a paddle 204 and an impeller 205. The motor 201 is fixed at the top of the tank body 1, the transmission shaft 202 is connected to the output shaft of the motor 201, the other end of the transmission shaft 202 is inserted into the tank body 1, the transmission shaft 202 is sealed and rotatably connected to the top of the tank body 1, the bottom end of the tank body 1 is a hemispherical structure, the connecting rod 203 is fixed to the bottom end of the transmission shaft 202, the connecting rod 203 is fixedly connected to the paddle 204 through a reinforcer 206, and the impeller 205 is fixed on the connecting rod 203.

[0057] A leak prevention device is provided at the connection between the transmission shaft 202 and the tank body 1, and its high-temperature resistance can meet the usage requirements. The paddle 204 cooperates with the bottom of the tank body 1. During the reaction, basically all the raw materials deposited at the bottom will be stirred, and the problem that some raw materials accumulate at the joints of the tank body 1 will not occur. Both the impeller 205 and the paddle 204 are for making the reaction proceed more smoothly and improving the reaction efficiency.

[0058] The blanking assembly 5 includes a blanking pipe 501, a hydraulic cylinder B502, a connector 503, a sealing ring 504, a concentric sleeve 505 and a discharge pipe 506. The blanking pipe 501 is fixedly installed at the central position of the bottom of the tank body 1. The blanking pipe 501 is communicated with the inside of the tank body 1. The top end of the blanking pipe 501 extends into the inside of the tank body 1 and is flush with the inner bottom wall of the tank body 1. The hydraulic cylinder B502 is inserted into the bottom end of the blanking pipe 501, and the connector 503 fixedly connects the two. The sealing ring 504 seals the outer wall of the hydraulic cylinder B502 and the inner wall of the blanking pipe 501. A sealing plug 507 is fixedly installed on the output shaft of the hydraulic cylinder B502, and the outer ring of the sealing plug 507 seals and slides with the inner wall of the blanking pipe 501;

[0059] A plurality of discharge holes 508 are provided on the side wall of the blanking pipe 501. The concentric sleeve 505 is fixedly sleeved outside the blanking pipe 501. The discharge holes 508 are communicated with the inside of the concentric sleeve 505. The discharge pipe 506 is fixed to and communicated with one side of the concentric sleeve 505. When the sealing plug 507 moves to the lowest position, it is below the discharge holes 508.

[0060] The function of the hydraulic cylinder B502 is the same as that of the hydraulic cylinder A402, which is to meet the sealing of the tank body 1 in a high-temperature and high-pressure environment, and can also quickly open the tank body 1 to connect the tank body 1 with the outside. Finally, the discharge pipe 506 is connected to a pump and a pipeline and then connected to the next neutralization reactor.

[0061] To ensure the arc flatness of the bottom of the tank body 1, in an alternative embodiment, as Figure 8 shown, the nitrogen replenisher 6 is located at the bottom end of the tank body 1. There are three nitrogen replenishers 6. The end connected to the tank body 1 extends into the bottom end inside of the tank body 1 and fits the arc surface of the inner wall of the bottom end of the tank body 1.

[0062] To ensure the arc flatness of the bottom of the tank body 1, in an alternative embodiment, as Figure 8 shown, the top surface of the sealing plug 507 is an arc-shaped groove structure, and when the sealing plug 507 extends to the uppermost end, it is flush with the inner wall of the lower end of the tank body 1, forming a complete spherical surface.

[0063] The spiral tube 301 surrounds the transmission shaft 202. The spiral tube 301 is located in the middle of the tank body 1 and is suspended. The spiral tube 301 is divided into an outer spiral part 3011 and an inner spiral part 3012. The inner spiral part 3012 is inside the outer spiral part 3011, and there is an equidistant gap between them. The ends of the outer spiral part 3011 and the inner spiral part 3012 far from the tank body 1 are both fixed to the joint 302. The inner spiral part 3012 is connected to the condenser and the vacuum unit through the joint 302 for cooling the inner spiral part 3012 and pumping air.

[0064] The suspended spiral tube 301 is more convenient for sucking the water vapor inside the tank body 1 and will not carry away the raw materials. Moreover, the double-layer structure makes the inner spiral part 3012 not easily affected by the temperature of the inner wall of the tank body 1. When the inner spiral part 3012 is connected to the condenser, due to the heat conduction performance of copper, the temperature of the inner spiral part 3012 is lower the farther it is from the tank body 1. Thus, the high-temperature water vapor will gradually condense into water droplets and adhere to the inner spiral part 3012. And the gas inside the tank body 1 is pumped from above, and nitrogen is continuously supplied from below. Therefore, the condensed water droplets will suspend in the middle of the tank body 1, which can be separated from the raw materials and will not return to the raw materials again. When continuously pumping air, the raw materials and water can be separated to the maximum extent.

[0065] The upper end of the tank body 1 is a hemispherical structure. The negative pressure air extraction pipe 7 and the nitrogen gas injection pipe 8 are both installed on this hemispherical structure.

[0066] In order to ensure smoother stirring of the materials and prevent the materials from getting stuck in the gap easily, in an alternative embodiment, as Figure 8 shown, the paddle 204 is an arc-shaped structure. The outer shape of the paddle 204 is the same as the outer shape of the bottom of the tank body 1, and the bottom end of the paddle 204 is attached to the inner wall of the bottom of the tank body 1.

[0067] During use

[0068] 1. Raw material preparation: Polyether diol, such as polytetrahydrofuran (PTMG). Dicarboxylic acid or anhydride, such as terephthalic acid (PTA) or adipic acid. Catalyst: Commonly used titanate or tin-based catalysts. Additives, such as antioxidants, stabilizers, etc. When adding raw materials and catalysts, the connecting shaft 403 is withdrawn by the hydraulic cylinder A402, so that the esterifying agent or raw materials are placed between the two pistons 404. When the connecting shaft 403 is pressed in, the two pistons 404 cooperate with the feeding pipe 401 to seal the esterifying agent. As one piston 404 enters the inside of the tank body 1, the esterifying agent will automatically fall into the tank body 1. During the adding process, only a very small amount of external gas enters the tank body 1. Before the prepolymerization reaction, all raw materials are mixed in proportion, and air is evacuated through the negative pressure exhaust pipe 7. At this time, multiple nitrogen replenishers 6 will replenish nitrogen into the inside of the tank body 1 from the bottom. After a period of circulation, the tank body 1 is basically completely filled with nitrogen. At this time, the reaction state using heating is carried out under complete nitrogen protection. If pressurization is required, nitrogen is further pressed in through the nitrogen pressure inlet pipe 8. Before that, the tank body 1 should be completely filled with nitrogen.

[0069] 2. Prepolymerization reaction

[0070] Mixing: Mix the polyether diol and dicarboxylic acid in proportion. The motor 201 can drive the transmission shaft 202 to rotate the paddle 204 at the bottom. The paddle 204 can accelerate the mixing between raw materials, and the impeller 205 will also rotate under the action of the transmission shaft 202, which can further mix the raw materials.

[0071] Heating: Under nitrogen protection, the inside of the tank body 1 is heated to 150 - 200 °C by the one-way heater 9.

[0072] 3. Removal of by-products

[0073] Dehydration: Remove the generated water by decompression or introducing inert gas to promote the reaction. After the reaction for a period of time, the pressure inside the tank body 1 can be reduced by evacuating through the exhaust pipe. After the pressure reduction, water molecules condense into steam. At this time, the spiral pipe 301 continuously evacuates the gas outward, and the nitrogen pressure inlet pipe 8 cooperates with it to further replenish dry nitrogen into the tank body 1 to keep the pressure constant inside the tank body 1. When the spiral pipe 301 continuously evacuates the gas, the gas circulates along the spiral pipe 301. The other end of the spiral pipe 301 is connected to a condenser, so the temperature gradually decreases along the pipe body. Therefore, water molecules can be condensed during continuous evacuation.

[0074] Reaction: Carry out esterification reaction to generate low molecular weight prepolymer and water.

[0075] 4. Further polymerization

[0076] Temperature increase: Raise the temperature to 250 - 280 °C.

[0077] Polycondensation: A polycondensation reaction is carried out under the action of a catalyst to form a high molecular weight polyether ester.

[0078] Vacuum reduction: Residual moisture is further removed under reduced pressure according to the above scheme.

[0079] 5. After the reaction is completed, the sealing state of the tank body 1 can be released by using the hydraulic cylinder B502, and the material after the reaction can be discharged through the blanking pipe 501 and the concentric sleeve 505.

[0080] In the description of this specification, the description with reference to terms such as "one embodiment", "some embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of this application. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine the different embodiments or examples described in this specification.

[0081] In addition, the technical solutions between various embodiments can be combined with each other, but it must be based on the ability of those of ordinary skill in the art to implement. When the combination of technical solutions results in contradictions or cannot be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection required by this application.

[0082] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A device for continuous production of polyether esters, comprising a dissolver, an esterification reactor, a neutralization reactor, a storage tank, a condenser and a plate-frame filter press. The raw materials are passed through the dissolver, the esterification reactor, the neutralization reactor, the esterification reactor and the plate-frame filter press to generate products into the storage tank. The condenser is used to discharge the water in the esterification reactor and the neutralization reactor, and is characterized in that: The esterification reactor comprises a tank body (1), a stirring assembly (2), a water vapor exhaust assembly (3), a feeding assembly (4) and a feeding assembly (5); a plurality of nitrogen supplementers (6) are installed at the bottom of the tank body (1); a negative pressure exhaust pipe (7) and a nitrogen pressure inlet pipe (8) are installed on one side of the top of the tank body (1); and the outer ring of the tank body (1) is covered with a one-way heater (9) for heating the tank body (1); The water vapor exhaust component (3) is installed inside the tank body (1), and the water vapor exhaust component (3) comprises a spiral tube (301) and a joint (302), the joint (302) penetrates the tank body (1) and the one-way heater (9), the spiral tube (301) is arranged inside the tank body (1) and is coaxial with the tank body (1), and the spiral tube (301) is connected and communicated with the joint (302); The feeding assembly (4) is installed on one side of the upper end of the tank body (1). The feeding assembly (4) comprises a feeding pipe (401), a hydraulic cylinder A (402), a connecting shaft (403) and a piston (404). The feeding pipe (401) is installed on the upper end of the tank body (1) and is connected to the interior thereof. Two pistons (404) are provided and are both fixed on the connecting shaft (403). The pistons (404) slide in a sealed manner with the inner wall of the feeding pipe (401). The hydraulic cylinder A (402) is fixed to the outer wall of the feeding pipe (401). The output shaft of the hydraulic cylinder A (402) is fixed to one end of the connecting shaft (403) outside the feeding pipe (401).

2. The device for continuous production of polyether esters according to claim 1, characterized in that: The stirring assembly (2) comprises a motor (201), a transmission shaft (202), a connecting rod (203), a paddle (204) and an impeller (205); the motor (201) is fixed at the top of the tank body (1); the transmission shaft (202) is connected to the output shaft of the motor (201); the other end of the transmission shaft (202) is inserted into the tank body (1); the transmission shaft (202) is sealingly rotatably connected to the top of the tank body (1); the bottom end of the tank body (1) is a hemispherical structure; the connecting rod (203) is fixed to the bottom end of the transmission shaft (202); the connecting rod (203) is fixedly connected to the paddle (204) via a reinforcer (206); and the impeller (205) is fixed to the connecting rod (203).

3. The device for continuous production of polyether ester according to claim 1, characterized in that: The material discharge assembly (5) comprises a material discharge pipe (501), a hydraulic cylinder B (502), a connector (503), a sealing ring (504), a concentric sleeve (505) and a discharge pipe (506); the material discharge pipe (501) is fixedly installed at the bottom center of the tank body (1); the material discharge pipe (501) is communicated with the interior of the tank body (1); the top end of the material discharge pipe (501) extends to the interior of the tank body (1) and is flush with the inner bottom wall of the tank body (1); the hydraulic cylinder B (502) is inserted into the bottom end of the material discharge pipe (501); the connector (503) is fixedly connected to the two; the sealing ring (504) seals the outer wall of the hydraulic cylinder B (502) and the inner wall of the material discharge pipe (501); the output shaft of the hydraulic cylinder B (502) is fixedly installed with a sealing plug (507); the outer ring of the sealing plug (507) slides in a sealing manner with the inner wall of the material discharge pipe (501); The side wall of the feed tube (501) is provided with a plurality of discharge holes (508); the concentric sleeve (505) is fixedly sleeved on the outside of the feed tube (501); the discharge holes (508) are connected with the inside of the concentric sleeve (505); the discharge pipe (506) is fixed to one side of the concentric sleeve (505) and is connected with the concentric sleeve (505); and the sealing plug (507) is located below the discharge hole (508) when it moves to the lowest position.

4. The device for continuous production of polyether ester according to claim 1, characterized in that: The nitrogen replenisher (6) is located at the bottom end of the tank body (1). Three nitrogen replenishers (6) are provided, and one end of the nitrogen replenisher (6) connected to the tank body (1) extends to the inside of the bottom end of the tank body (1) and fits with the arc surface of the inner wall of the bottom end of the tank body (1).

5. The device for continuous production of polyether ester according to claim 3, characterized in that: The top surface of the sealing plug (507) is an arc-shaped groove structure, and when the sealing plug (507) extends to the uppermost end, it is flush with the inner wall of the lower end of the tank body (1), forming a complete spherical surface.

6. The device for continuous production of polyether ester according to claim 2, characterized in that: The spiral tube (301) surrounds the transmission shaft (202), the spiral tube (301) is located in the middle of the tank body (1), and the spiral tube (301) is suspended in the air; The spiral tube (301) is divided into an outer spiral portion (3011) and an inner spiral portion (3012). The inner spiral portion (3012) is located inside the outer spiral portion (3011), and there is an equidistant gap between the two. The ends of the outer spiral portion (3011) and the inner spiral portion (3012) away from the tank body (1) are both fixed to a joint (302). The inner spiral portion (3012) is connected to a condenser and a vacuum unit via the joint (302) for cooling the inner spiral portion (3012) and extracting air.

7. The device for continuous production of polyether ester according to claim 1, characterized in that: The upper end of the tank body (1) is a hemispherical structure, and the negative pressure exhaust pipe (7) and the nitrogen pressure inlet pipe (8) are both installed on the hemispherical structure.

8. The device for continuous production of polyether esters according to claim 2, characterized in that: The paddle (204) is an arc-shaped structure, the shape of the paddle (204) is the same as the shape of the bottom of the tank body (1), and the bottom end of the paddle (204) fits against the inner wall of the bottom of the tank body (1).

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