Special supergravity filler suitable for devolatilization of high-viscosity polymer, supergravity rotary devolatilization device and high-viscosity polymer devolatilization system

Abstract

The invention discloses a special supergravity filler suitable for devolatilization of a high-viscosity polymer, a supergravity rotary devolatilization device and a high-viscosity polymer devolatilization system. The filler is of a three-layer structure, the first layer is filler of a blade-shaped structure, the second layer is 3D printing filler, and the third layer is silk screen filler. The special supergravity filler suitable for devolatilization of the high-viscosity polymer, provided by the invention, is filled in a supergravity rotary devolatilization device, and can cut a polymer solution into liquid filaments, liquid films and liquid drops with extremely small sizes under the strong shearing force of the rotary filler, so that the surface exposure area of the polymer is increased, and the devolatilization of the high-viscosity polymer is facilitated. The surface updating speed is accelerated, and the diffusion distance of volatile components in the polymer is shortened; meanwhile, the apparent viscosity of the polymer is reduced, bubble breakage is facilitated and the like, so that the mass transfer process of polymer devolatilization is enhanced, and the devolatilization efficiency is improved; the method has the advantages of high devolatilization efficiency, thorough volatile component removal, short time, low energy consumption, small equipment size and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of special filler of high gravity for high viscosity polymer devolatilization, high gravity rotary devolatilization device, high viscosity polymer devolatilization system and the method for removing volatile component in polymer of high gravity, belong to the technical field of removing volatile component in polymer. BACKGROUND

[0002] Polymer is an important product in chemical production process, in the polymer processing production process, there are some unexpected low molecular weight components in the polymer product from the reactor, such as monomer, solvent, water, even by-product. These components are called volatile, which can have a negative impact on the characteristics and performance of the product, and even harm to the environment and the health of users. Therefore, it is essential to remove or recover residual components from the polymer. Polymer devolatilization is a process for removing volatile components from polymer products, which is a key technology for polymer production and processing. The importance of polymer devolatilization in the polymerization process is only second to the polymerization process formulation and mixing unit operation.

[0003] At present, the polymer devolatilization method and device can be divided into static and dynamic types. Static devolatilization relies on gravity to transport polymer in the devolatilization zone. The static devolatilization device commonly used in industry is mainly flash evaporator, falling strip devolatilizer, etc. Dynamic devolatilization device is divided into thin film renewal type devolatilization device, extrusion type devolatilization device and surface renewal type devolatilization device. In the polymer devolatilization industry, the devolatilization equipment is mainly surface renewal type devolatilization device.

[0004] The design of the devolatilization equipment requires not only to provide a large mass transfer specific surface area, but also to ensure that the material flows continuously and is mixed to enhance the polymer surface renewal as much as possible; in addition, the residence time of the material in the devolatilization device should be uniform and controllable to obtain the required devolatilization effect. Therefore, the ideal devolatilization device should meet the requirements of flat flow, no dead zone, maximum mass transfer area per unit time (film forming efficiency), fast surface renewal and short small molecule diffusion path. The currently disclosed high viscosity material devolatilization equipment includes disc type and cage type, both of which are horizontal mixers. These two types of equipment are driven by rotating devices immersed in the material, which can bring the melt material up to form a film for devolatilization. This method has low melt film forming efficiency, limited surface renewal, especially when the viscosity is high, it is difficult to devolatilize, and the film forming is uneven, which makes the devolatilization effect poor; in addition, when the viscosity is high, the energy consumption required for rotation increases sharply. Therefore, it is urgent to develop a devolatilization device with large film forming area, controllable film forming shape, no dead zone, fast surface renewal, uniform and controllable residence time in film forming process, large flow range adaptability and low energy consumption.

[0005] Chinese patent CN101372522A discloses a method for removing volatile components from polymers. In a high-gravity rotating bed devolatilization device, heated liquid polymer is transported to the hollow cavity of the rotor packing. Under centrifugal force, it passes through a rotating packed bed, and the devolatilization process occurs within the rotating packing layer. The high-gravity rotating bed devolatilization device is maintained at a vacuum of 0-760 mmHg, causing the liquid polymer to be vertically and evenly distributed in layers along the axial direction within the hollow cavity of the packing. The rotor speed is adjusted to achieve a high-gravity level of 30-1000g. Different shapes and types of annular packing are filled at intervals along the diameter of the packing core, arranged in a concentric multi-layered shaped packing. The liquid polymer flows from the inner cavity to the outer edge of the packing according to the customized path of the multi-layered shaped packing. The method uses a concentric multi-layered shaped packing arranged in the order of inward-grid-outward-grid packing. However, the inward and outward inward structures of this packing can obstruct polymer flow, resulting in poor devolatilization performance.

[0006] As a core component of a rotating devolatilization apparatus in high gravity, the packing material plays a crucial role in mass transfer and devolatilization within the apparatus. The packing structure has a particularly significant impact on the devolatilization and mass transfer performance of the apparatus, and its performance can be improved by altering the packing structure. Structured packing exhibits good homogeneity and can still achieve mixing and dispersion between phases in a high-speed rotating high-gravity apparatus. Therefore, the design and development of novel packing materials is essential for enhancing the mass transfer performance of high-gravity devolatilization apparatuses. Summary of the Invention

[0007] The present invention aims to provide a special filler for high-viscosity polymer devolatilization, a high-gravity rotary devolatilization device, a high-viscosity polymer devolatilization system, and a method for removing volatiles from polymers by high gravity, thereby increasing the effective film-forming area of ​​the material and improving the surface renewal rate and devolatilization efficiency of the material.

[0008] To achieve the above objectives, the present invention provides a special filler for high-gravity polymer devolatilization, wherein the filler has a three-layer structure, the first layer is a blade-shaped filler, the second layer is a 3D-printed filler, and the third layer is a wire mesh filler.

[0009] The present invention relates to a special filler for high-gravity polymer devolatilization, wherein the filler is annular, and the first layer is located in the inner layer, the second layer is located in the middle layer, and the third layer is located in the outer layer.

[0010] The present invention provides a special filler for high-gravity polymer devolatilization, wherein the radial width ratio of the first layer, the second layer, and the third layer is 1:1:1 to 1:5:10; the pore size of the first layer, the second layer, and the third layer decreases sequentially; and the pore size of the wire mesh filler is 2 to 6 mm.

[0011] The present invention provides a special filler for high-viscosity polymer devolatilization, wherein the blade-shaped filler has one, two, or multiple layers.

[0012] When the number of layers of the blade-shaped packing is two or more, the two or more layers of the blade-shaped packing are staggered.

[0013] The blade-shaped packing is inclined at an angle of 5 to 30°.

[0014] The blade-shaped packing material is also provided with an opening, the diameter of which is d, where d is 5-8 mm;

[0015] The shape of the opening is at least one of the following: circular, square, and rhomboid.

[0016] The present invention provides a special filler for high-gravity polymer devolatilization, wherein the blade-structured filler has fins installed near the opening on the inner edge, and the size of the fins is equivalent to the size of the opening.

[0017] The shape of the fins is at least one of the following: circular, rectangular, rhomboid, and wavy.

[0018] The present invention relates to a special filler for high-viscosity polymer devolatilization under ultragravity conditions. The 3D printed filler is a filler with multiple pore structures distributed in a shape of at least one of circular, square, and rhomboid. The multiple pore structures are staggered (d / 3-d / 2) inside the 3D printed filler.

[0019] The present invention provides a special filler for high-viscosity polymer devolatilization under ultragravity conditions. The lower half of the 3D printed filler is further provided with one, two or more cylindrical baffles. The height of the cylindrical baffles is 30 to 50% of the height of the 3D printed filler. The shape of the cylindrical baffles is at least one of the following: annular, wavy, and inverted conical.

[0020] The present invention also provides a supergravity rotational devolatilization device, which includes: a housing, a rotor, a sealing device, a liquid distributor, and a drive mechanism; the rotor is filled with the aforementioned packing material, and the rotor is located inside the housing; the top center of the housing has a liquid inlet, which is connected to the liquid distributor, which is located at the center of the packing material inside the rotor; the bottom of the housing has a liquid outlet; the drive mechanism is connected to the rotor and is used to drive the rotor to rotate; the sealing device is used to ensure the sealing performance of the supergravity rotational devolatilization device.

[0021] The supergravity rotational devolatilization device of the present invention has a jacket on the outside of the shell, the jacket being used to heat the supergravity rotational devolatilization device; the shell also has a pressure relief port.

[0022] The supergravity rotational devouring device of the present invention includes a driving mechanism comprising a rotating shaft and a motor; the upper end of the rotating shaft is fixedly connected to the rotor, and the lower end of the rotating shaft is connected to the motor through a bearing, thereby realizing the rotation of the rotor under the drive of the motor.

[0023] The supergravity rotation devouring device of the present invention includes a sealing device comprising at least one of a shaft seal, an O-ring, and an oil seal.

[0024] The present invention also provides a high-viscosity polymer devolatilization system, the devolatilization system comprising a supergravity rotary devolatilization device, a vacuum unit and a feeding unit; the supergravity rotary devolatilization device has a rotor filled with the above-mentioned filler at its center; the feeding unit is connected to the liquid inlet of the supergravity rotary devolatilization device, and the vacuum unit is connected to the liquid outlet of the supergravity rotary devolatilization device.

[0025] The high-viscosity polymer devolatilization system of the present invention includes a vacuum unit comprising: a vacuum pump, a piezoresistive vacuum gauge, a discharge liquid storage tank, a condenser, a gas-liquid separator, and an adsorption tank; the vacuum pump is a rotary vane vacuum pump; the discharge liquid storage tank can withstand a high vacuum degree, and has four ports at the top and a discharge port at the bottom; one port at the top of the discharge liquid storage tank is connected to the liquid outlet at the bottom of the high-gravity rotary devolatilization device, the discharge liquid storage tank is connected to the condenser, and another port at the top of the discharge liquid storage tank is also connected to a connection port on the side wall of the shell of the high-gravity rotary devolatilization device to maintain a constant vacuum degree in the devolatilization system, in which case the discharge liquid storage tank acts as a buffer tank; the condenser is connected to the top of the gas-liquid separator, one side of the gas-liquid separator is connected to the top of the adsorption tank, and the bottom of the adsorption tank is connected to the vacuum pump.

[0026] The high-viscosity polymer devolatilization system of the present invention includes an adsorption tank filled with 5A molecular sieves or activated carbon to adsorb uncondensed volatiles.

[0027] The high-viscosity polymer devolatilization system of the present invention includes a feeding unit comprising: a melting tank, a raw material liquid storage tank, and a gear pump; the melting tank is used for melting the polymer, the top of the raw material liquid storage tank is provided with a feed inlet and a vent, and the bottom of the raw material liquid storage tank is provided with a discharge outlet; the feed inlet of the raw material liquid storage tank is connected to the melting tank, and the discharge outlet of the raw material liquid storage tank is connected to the gear pump; the gear pump is a gear metering pump suitable for conveying high-viscosity media; the gear pump is connected to the liquid inlet of the high-gravity rotary devolatilization device, and a flow meter is also provided between the gear pump and the high-gravity rotary devolatilization device.

[0028] This invention further provides a method for removing volatiles from polymers using ultragravity, the method comprising the following steps:

[0029] (1) Add the polymer solution containing volatiles to the raw material storage tank;

[0030] (2) Turn on the vacuum pump to bring the entire system into a vacuum state;

[0031] (3) Activate the hypergravity rotation devouring device: turn on the motor and set the hypergravity factor;

[0032] (4) Start the gear pump and inject the polymer solution into the gravity rotary devolatilization device through the inlet;

[0033] (5) Determination of volatile content: After the polymer solution is treated by the supergravity rotary devolatilization device, a sample is taken from the outlet to detect the volatile content.

[0034] In the method for removing volatiles from polymers by supergravity of the present invention, in step (2), the vacuum degree of the entire system is 0.08 to 0.095 MPa.

[0035] In the method for removing volatiles from polymers by supergravity of the present invention, in step (3), the supergravity factor is set to 30-90, preferably 60-80.

[0036] The present invention relates to a method for removing volatiles from polymers using ultragravity, wherein the temperature of the polymer solution is 25–160°C, the mass content of the volatiles is 5%–20%, and the flow rate of the polymer solution is 0.1–1.5 m / s.

[0037] Compared with existing technologies, the supergravity-specific packing material provided by this invention, suitable for the devolatilization of high-viscosity polymers, is filled in a supergravity rotary devolatilization device. Under the strong shear force of the rotating packing material, the polymer solution can be cut into extremely small liquid filaments, liquid films, and droplets. This increases the exposed surface area of ​​the polymer, accelerates the surface renewal rate, and shortens the diffusion distance of volatiles in the polymer. At the same time, it reduces the apparent viscosity of the polymer and facilitates bubble rupture, thereby enhancing the mass transfer process of polymer devolatilization and improving the devolatilization efficiency. This invention has the advantages of high devolatilization efficiency, thorough removal of volatiles, short time, low energy consumption, and small equipment size. Attached Figure Description

[0038] Figure 1 This is a schematic diagram of the structure of the special packing material of the present invention.

[0039] Figure 2 This is a schematic diagram of the structure of the first, second, and third layers of the packing material of the present invention.

[0040] Figure 3This is a schematic diagram of the 3D printed filler and cylindrical baffle of the present invention.

[0041] Figure 4 This is a schematic diagram of the high-viscosity polymer devolatilization system of the present invention.

[0042] In the attached figures, the following labels are used:

[0043] 100-packing

[0044] 101 - First Floor

[0045] 102 - Second Floor

[0046] 102-1-Cylindrical baffle

[0047] 103 - Third Floor

[0048] 1-Melting tank

[0049] 2-Raw material storage tank

[0050] 3-Gear Pump

[0051] 4-Flowmeter

[0052] 5-Supergravity Rotary Deviation Device

[0053] 501-Inlet

[0054] 502-Liquid Distributor

[0055] 503-Liquid outlet

[0056] 504-Connector

[0057] 505-Drive Mechanism

[0058] 506 - Sealing Device

[0059] 507 - Housing

[0060] 508-rotor

[0061] 509-Pressure relief port

[0062] 6-Discharge liquid storage tank

[0063] 7-Condenser

[0064] 8-Gas-Liquid Separator

[0065] 9-Adsorption tank

[0066] 10-Vacuum Pump Detailed Implementation

[0067] The present invention will be further described below with reference to the accompanying drawings.

[0068] Figure 1 This is a schematic diagram of the structure of the special packing material of the present invention. Figure 2 This is a schematic diagram of the structure of the first, second, and third layers of the packing material of the present invention. Please also refer to... Figure 2 The filler 100 has a three-layer structure: the first layer 101 is a blade-shaped filler, the second layer 102 is a 3D printed filler, and the third layer 103 is a wire mesh filler.

[0069] Furthermore, the filler 100 is annular, with the first layer 101 located in the inner layer, the second layer 102 located in the middle layer, and the third layer 103 located in the outer layer.

[0070] Furthermore, the radial width ratio of the first layer 101, the second layer 102, and the third layer 103 is 1:1:1 to 1:5:10; the aperture of the first layer 101, the second layer 102, and the third layer 103 decreases sequentially; the aperture of the wire mesh filler in the third layer 103 is 2 to 6 mm.

[0071] Furthermore, the number of layers of the blade-shaped packing is single, two, or multiple; when the number of layers of the blade-shaped packing is two or more, the two or more layers of blade-shaped packing are staggered; the blade-shaped packing is inclined, with an inclination angle of 5 to 30°; the blade-shaped packing also has openings, the diameter of which is d, where d is 5-8 mm; the shape of the openings is at least one of circular, square, and rhomboid.

[0072] Furthermore, the filler of the blade structure is fitted with fins near the opening on the inner edge, and the size of the fins is comparable to the size of the opening; the shape of the fins is at least one of circular, rectangular, rhomboid, and wavy.

[0073] Further, please refer to Figure 2 The 3D printing filler is a filler with multiple pore structures, and the shape of the pore structure is at least one of circular, square, and rhomboid; the multiple pore structures are staggered (d / 3-d / 2) inside the 3D printing filler.

[0074] Further, please refer to Figure 3 , Figure 3 The diagram shows the structure of the 3D printing filler and cylindrical baffle of the present invention. The lower half of the 3D printing filler is provided with one, two or more cylindrical baffles 102-1. The height of the cylindrical baffle 102-1 is 30 to 50% of the height of the 3D printing filler. The shape of the cylindrical baffle 102-1 is at least one of the following: annular, wavy, and inverted conical.

[0075] Figure 4This is a schematic diagram of the high-viscosity polymer devolatilization system of the present invention. The supergravity rotary devolatilization device 5 of the present invention includes: a housing 507, a rotor 508, a sealing device 506, a liquid distributor 502, and a drive mechanism 505; the rotor 508 is filled with packing material 100 and is located inside the housing 507. The top center of the housing 507 has a liquid inlet 501, which is connected to the liquid distributor 502. The liquid distributor 502 is located at the center of the packing material 100 inside the rotor 508; the bottom of the housing 507 has a liquid outlet 503; the drive mechanism 505 is connected to the rotor 508 and is used to drive the rotor 508 to rotate; the sealing device 506 is used to ensure the sealing performance of the supergravity rotary devolatilization device 5.

[0076] Furthermore, the outer shell 507 of the supergravity rotational devouring device 5 is provided with a jacket, which is used to heat the supergravity rotational devouring device 5; the shell 507 is also provided with a pressure relief port 509.

[0077] Furthermore, the drive mechanism 505 includes a rotating shaft and a motor; the upper end of the rotating shaft is fixedly connected to the rotor, and the lower end of the rotating shaft is connected to the motor through a bearing, so that the rotor can rotate under the drive of the motor.

[0078] Furthermore, the sealing device includes at least one of shaft seal, O-ring, and oil seal.

[0079] Please continue to refer to Figure 4 The high-viscosity polymer devolatilization system of the present invention includes a high-gravity rotary devolatilization device 5, a vacuum unit and a feeding unit; the high-gravity rotary devolatilization device 5 has a rotor filled with packing material 100 at its center; the feeding unit is connected to the liquid inlet of the high-gravity rotary devolatilization device 5 and the vacuum unit is connected to the liquid outlet of the high-gravity rotary devolatilization device 5.

[0080] Furthermore, the vacuum unit includes: a vacuum pump 10, a piezoresistive vacuum gauge, a discharge liquid storage tank 6, a condenser 7, a gas-liquid separator 8, and an adsorption tank 9; the vacuum pump 10 is a rotary vane vacuum pump; the discharge liquid storage tank 6 can withstand a high vacuum degree, and the top of the discharge liquid storage tank 6 is provided with four ports, and the bottom of the discharge liquid storage tank 6 is provided with a discharge port; one port at the top of the discharge liquid storage tank 6 is connected to the liquid outlet 503 at the bottom of the supergravity rotary devolatilization device 5, the discharge liquid storage tank 6 is connected to the condenser 7, and the other port at the top of the discharge liquid storage tank 6 is also connected to the connection port 504 on the side wall of the shell of the supergravity rotary devolatilization device 5 to maintain a constant vacuum degree in the devolatilization system. At this time, the discharge liquid storage tank 6 acts as a buffer tank; the condenser 7 is connected to the top of the gas-liquid separator 8, one side of the gas-liquid separator 8 is connected to the top of the adsorption tank 9, and the bottom of the adsorption tank 9 is connected to the vacuum pump 10.

[0081] Furthermore, the adsorption tank 9 is filled with 5A molecular sieves or activated carbon to adsorb the volatiles that have not condensed.

[0082] Furthermore, the feeding unit includes: a melting tank 1, a raw material liquid storage tank 2, and a gear pump 3; the melting tank 1 is used for melting the polymer, the top of the raw material liquid storage tank 2 is provided with a feed inlet and a vent, and the bottom of the raw material liquid storage tank 2 is provided with a discharge outlet; the feed inlet of the raw material liquid storage tank 2 is connected to the melting tank 1, and the discharge outlet of the raw material liquid storage tank 2 is connected to the gear pump 3; the gear pump 3 is a gear metering pump suitable for conveying high-viscosity media; the gear pump 3 is connected to the liquid inlet 501 of the high-gravity rotary devolatilization device 5, and a flow meter 5 is also provided between the gear pump 3 and the high-gravity rotary devolatilization device 5.

[0083] This invention further provides a method for removing volatiles from polymers using ultragravity, the method comprising the following steps:

[0084] (1) Add the polymer solution containing volatiles to the raw material storage tank 2;

[0085] (2) Turn on the vacuum pump to bring the entire system into a vacuum state;

[0086] (3) Activate the hypergravity rotation devouring device 5: turn on the motor and set the hypergravity factor;

[0087] (4) Start the gear pump and inject the polymer solution into the super gravity rotary devolatilization device 5 through the inlet 501;

[0088] (5) Determination of volatile content: After the polymer solution is treated by the supergravity rotating devolatilization device 5, a sample is taken from the outlet to detect the volatile content.

[0089] Furthermore, in step (2), the vacuum degree of the entire system is 0.08-0.095 MPa.

[0090] Furthermore, in step (3), the hypergravity factor is set to 30-90, preferably 60-80.

[0091] Furthermore, the temperature of the polymer solution is 25–160°C, and the mass content of volatile matter is 5%–20%; the flow rate of the polymer solution is 0.1–1.5 m / s.

[0092] The present invention will be described in detail below with reference to the embodiments. The embodiments are implemented under the premise of the technical solution of the present invention, and detailed implementation methods and processes are given. However, the protection scope of the present invention is not limited to the following embodiments. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions.

[0093] Example 1

[0094] Adopting such Figure 4The high-viscosity polymer devolatilization system shown is used for devolatilization treatment. The rotor of the high-gravity rotating devolatilization device is filled with packing material. The packing material has a three-layer structure. The radial width ratio of the first, second, and third layers is 1:1:1, and the pore size of the first, second, and third layers decreases sequentially.

[0095] The first layer is a single layer of blade-shaped packing. The blade-shaped packing is angled at 5° and has openings with a diameter (d) of 5mm. Circular fins are installed near the inner edge of the openings.

[0096] The second layer is 3D printed filler, which has multiple circular hole structures distributed inside the 3D printed filler. The multiple circular hole structures are staggered inside the 3D printed filler. The lower half of the 3D printed filler is also equipped with a cylindrical baffle. The height of the cylindrical baffle is 30% of the height of the 3D printed filler, and the shape of the cylindrical baffle is circular.

[0097] The third layer is a wire mesh filler with a pore size of 2mm.

[0098] (1) After adding the POE-cyclohexane polymer solution containing volatile cyclohexane to the melting tank and preheating it to 110°C, it is placed in the raw material storage tank. The volatile cyclohexane mass content is 15.15%.

[0099] (2) Turn on the vacuum pump to make the vacuum level of the entire system 0.084 to 0.086 MPa;

[0100] (3) Activate the hypergravity rotation and devouring device: turn on the motor and set the hypergravity factor to 60;

[0101] (4) Start the gear pump and input the POE-cyclohexane polymer solution into the gravity rotary devolatilization device through the inlet. The flow rate of the polymer solution is 0.2 m / s.

[0102] (5) Determination of volatile content: After the polymer solution was treated by the centrifugal rotary devolatilization device, a sample was taken from the outlet and the volatile content of cyclohexane was found to be 0.0267%.

[0103] Example 2

[0104] Adopting such Figure 4 The high-viscosity polymer devolatilization system shown is used for devolatilization treatment. The rotor of the high-gravity rotating devolatilization device is filled with packing material. The packing material has a three-layer structure. The radial width ratio of the first, second, and third layers is 1:2:2, and the pore size of the first, second, and third layers decreases sequentially.

[0105] The first layer is a blade-shaped packing material, consisting of two layers that are staggered and inclined at a 10° angle. Each blade-shaped packing material has an opening with a diameter (d) of 6 mm and a square shape. Fins, which are rectangular in shape, are installed near the inner edge of the opening.

[0106] The second layer is 3D printed filler, which has multiple square hole structures distributed inside the 3D printed filler. The multiple square hole structures are staggered inside the 3D printed filler. The lower half of the 3D printed filler also has two cylindrical baffles. The height of the cylindrical baffles is 30% of the height of the 3D printed filler. One cylindrical baffle is ring-shaped and the other is wavy.

[0107] The third layer is a wire mesh filler with a pore size of 3mm.

[0108] (1) After adding the POE-cyclohexane polymer solution containing volatile cyclohexane to the melting tank and preheating it to 120°C, it is placed in the raw material storage tank. The volatile cyclohexane mass content is 9.53%.

[0109] (2) Turn on the vacuum pump to make the vacuum level of the entire system 0.084 to 0.09 MPa;

[0110] (3) Activate the hypergravity rotation and detachment device: turn on the motor and set the hypergravity factor to 70;

[0111] (4) Start the gear pump and input the POE-cyclohexane polymer solution into the gravity rotary devolatilization device through the inlet. The flow rate of the polymer solution is 0.3 m / s.

[0112] (5) Determination of volatile content: After the polymer solution was treated by the centrifugal rotary devolatilization device, a sample was taken from the outlet and the volatile cyclohexane content was found to be 0.0132%.

[0113] Example 3

[0114] Adopting such Figure 4 The high-viscosity polymer devolatilization system shown is used for devolatilization treatment. The rotor of the high-gravity rotating devolatilization device is filled with packing material. The packing material has a three-layer structure. The radial width ratio of the first, second, and third layers is 1:2:3, and the pore size of the first, second, and third layers decreases sequentially.

[0115] The first layer is a three-layer packing material with a blade-shaped structure. These three layers are staggered and angled at 15°. Each blade-shaped packing material has an opening with a diameter (d) of 5mm and a rhomboid shape. Fins, also rhomboid in shape, are installed near the inner edge of the opening.

[0116] The second layer is 3D printed filler, which has multiple rhomboid pore structures distributed inside the 3D printed filler. The multiple rhomboid pore structures are staggered inside the 3D printed filler. The lower half of the 3D printed filler also has 3 cylindrical baffles. The height of the cylindrical baffles is 50% of the height of the 3D printed filler. Two of the cylindrical baffles are in the shape of rings, and one cylindrical baffle is in the shape of an inverted cone.

[0117] The third layer is wire mesh filler with a pore size of 4mm.

[0118] (1) After adding the POE-cyclohexane polymer solution containing volatile cyclohexane to a melting tank and preheating it to 130°C, it is placed in a raw material storage tank. The volatile cyclohexane mass content is 19.53%.

[0119] (2) Turn on the vacuum pump to make the vacuum level of the entire system 0.084 to 0.086 MPa;

[0120] (3) Activate the hypergravity rotation and detachment device: turn on the motor and set the hypergravity factor to 80;

[0121] (4) Start the gear pump and input the POE-cyclohexane polymer solution into the gravity rotary devolatilization device through the inlet. The flow rate of the polymer solution is 0.5 m / s.

[0122] (5) Determination of volatile content: After the polymer solution is treated by the centrifugal rotary devolatilization device, a sample is taken from the outlet and the volatile cyclohexane content is found to be 0.0155%.

[0123] Example 4

[0124] Adopting such Figure 4 The high-viscosity polymer devolatilization system shown is used for devolatilization treatment. The rotor of the high-gravity rotating devolatilization device is filled with packing material. The packing material has a three-layer structure. The radial width ratio of the first, second, and third layers is 1:4:8, and the pore size of the first, second, and third layers decreases sequentially.

[0125] The first layer is a blade-shaped packing material, consisting of two layers that are staggered and inclined at a 30° angle. Each blade-shaped packing material has an opening with a diameter (d) of 7 mm and a circular shape. Fins, in a rhomboid shape, are installed near the inner edge of the opening.

[0126] The second layer is 3D printed filler, which has multiple circular hole structures distributed within it. These circular hole structures are staggered inside the 3D printed filler. The lower half of the 3D printed filler also has four cylindrical baffles, each with a height of 30% of the 3D printed filler height. One of the cylindrical baffles is annular, two are inverted conical, and one is wavy.

[0127] The third layer is a wire mesh filler with a pore size of 6mm.

[0128] (1) After adding the POE-cyclohexane polymer solution containing volatile cyclohexane to the melting tank and preheating it to 120°C, it is placed in the raw material storage tank. The volatile cyclohexane mass content is 19.53%.

[0129] (2) Turn on the vacuum pump to make the vacuum level of the entire system 0.084 to 0.086 MPa;

[0130] (3) Activate the hypergravity rotation devouring device: turn on the motor and set the hypergravity factor to 85;

[0131] (4) Start the gear pump and input the POE-cyclohexane polymer solution into the gravity rotary devolatilization device through the inlet. The flow rate of the polymer solution is 0.3 m / s.

[0132] (5) Determination of volatile content: After the polymer solution was treated by the centrifugal rotary devolatilization device, a sample was taken from the outlet and the volatile content of cyclohexane was found to be 0.016%.

[0133] Example 5

[0134] Adopting such Figure 4 The high-viscosity polymer devolatilization system shown is used for devolatilization treatment. The rotor of the high-gravity rotary devolatilization device is filled with packing material. The packing material has a three-layer structure. The radial width ratio of the first, second, and third layers is 1:3:9, and the pore size of the first, second, and third layers decreases sequentially.

[0135] The first layer is a three-layer packing material with a blade-shaped structure. These three layers are staggered and angled at 20°. Each blade-shaped packing material has an opening with a diameter (d) of 7mm and a square shape. Fins, in a rhomboid shape, are installed near the inner edge of the opening.

[0136] The second layer is 3D printed filler, which has multiple circular hole structures distributed within it. These circular hole structures are staggered inside the 3D printed filler. The lower half of the 3D printed filler also has two cylindrical baffles, each with a height of 40% of the 3D printed filler height. The two cylindrical baffles are inverted conical in shape.

[0137] The third layer is a wire mesh filler with a pore size of 6mm.

[0138] (1) After adding the POE-cyclohexane polymer solution containing volatile cyclohexane to a melting tank and preheating it to 120°C, it is placed in a raw material storage tank. The volatile cyclohexane mass content is 19.21%.

[0139] (2) Turn on the vacuum pump to make the vacuum level of the entire system 0.084 to 0.086 MPa;

[0140] (3) Activate the hypergravity rotation and detachment device: turn on the motor and set the hypergravity factor to 90;

[0141] (4) Start the gear pump and input the POE-cyclohexane polymer solution into the gravity rotary devolatilization device through the inlet. The flow rate of the polymer solution is 0.4 m / s.

[0142] (5) Determination of volatile content: After the polymer solution was treated by the centrifugal rotary devolatilization device, a sample was taken from the outlet and the volatile cyclohexane content was found to be 0.0174%.

[0143] Comparative Example 1

[0144] The only difference from Example 1 is that the first, second, and third layers of packing in the supergravity rotary devouring device are all blade-shaped packings; otherwise, they are the same as in Example 1.

[0145] After the polymer solution was treated by a high-gravity rotary devolatilization device, a sample was taken from the outlet. The volatile cyclohexane content was found to be reduced to only 2.8293%, which is much higher than the 0.0267% in Example 1.

[0146] Comparative Example 2

[0147] The only difference from Example 1 is that the first, second, and third layers of packing in the supergravity rotary devolatilization device are all wire mesh packing; otherwise, they are the same as in Example 1.

[0148] After the polymer solution was treated by a high-gravity rotary devolatilization device, a sample was taken from the outlet. The volatile cyclohexane content was found to be 1.5264%, which is much higher than the 0.0267% in Example 1.

[0149] Comparative Example 3

[0150] The only difference from Example 1 is that the packing in the supergravity rotary devouring device is the packing arranged in a regular pattern of inner inclined type-grid type-outer inclined type-grid type as shown in Example 2 of CN101372522A. Otherwise, it is the same as Example 1.

[0151] After the polymer solution was treated by a high-gravity rotary devolatilization device, a sample was taken from the outlet. The volatile cyclohexane content was found to be 1.2516%, which is significantly higher than the 0.0267% concentration in Example 1.

[0152] Comparative Example 4

[0153] The only difference from Example 3 is that the first, second, and third layers of packing in the supergravity rotary devolatilization device are all wire mesh packing; otherwise, they are the same as in Example 3.

[0154] After the polymer solution was treated by a high-gravity rotary devolatilization device, a sample was taken from the outlet. The volatile cyclohexane content was found to be 3.6475%, which is significantly higher than the 0.0185% concentration in Example 3.

[0155] As can be seen from the results of the examples and comparative examples, compared with the comparative examples, the high-viscosity polymer devolatilization system using the supergravity special packing of the present invention removes volatiles more thoroughly, and the present invention has a higher devolatilization efficiency.

[0156] Of course, the present invention may have other various embodiments. Without departing from the spirit and essence of the present invention, those skilled in the art can make various corresponding changes and modifications according to the present invention, but these corresponding changes and modifications should all fall within the protection scope of the present invention.

Claims

1. A special filler for high-gravity polymer devolatilization, characterized in that, The filler has a three-layer structure: the first layer is a blade-shaped filler, the second layer is a 3D-printed filler, and the third layer is a wire mesh filler.

2. The special filler for high-viscosity polymer devolatilization according to claim 1, characterized in that, The filler is annular, with the first layer located in the inner layer, the second layer in the middle layer, and the third layer in the outer layer.

3. The special filler for high-viscosity polymer devolatilization according to claim 2, characterized in that, The radial width ratio of the first layer, the second layer, and the third layer is 1:1:1 to 1:5:10; the pore size of the first layer, the second layer, and the third layer decreases sequentially; the pore size of the wire mesh filler is 2 to 6 mm.

4. The special filler for high-viscosity polymer devolatilization according to claim 1, characterized in that, The number of layers of the blade-shaped packing is single, two, or multiple; When the number of layers of the blade-shaped packing is two or more, the two or more layers of the blade-shaped packing are staggered. The blade-shaped packing is inclined at an angle of 5 to 30°. The blade-shaped packing material is also provided with an opening, the diameter of which is d, where d is 5-8 mm; The shape of the opening is at least one of the following: circular, square, and rhomboid.

5. The special filler for high-viscosity polymer devolatilization according to claim 4, characterized in that, The filler of the blade structure is also fitted with fins near the opening on the inner edge of the fin, and the size of the fins is equivalent to the size of the opening. The shape of the fins is at least one of the following: circular, rectangular, rhomboid, and wavy.

6. The special filler for high-viscosity polymer devolatilization according to claim 1, characterized in that, The 3D printing filler is a filler with multiple pore structures, and the shape of the pore structure is at least one of circular, square, and rhomboid; the multiple pore structures are staggered (d / 3-d / 2) inside the 3D printing filler.

7. The special filler for high-viscosity polymer devolatilization according to claim 1, characterized in that, The lower half of the 3D printing filler is further provided with one, two or more cylindrical baffles. The height of the cylindrical baffles is 30 to 50% of the height of the 3D printing filler. The shape of the cylindrical baffles is at least one of the following: annular, wavy, and inverted conical.

8. A supergravity rotational devouring device, characterized in that, include: The device comprises a housing, a rotor, a sealing device, a liquid distributor, and a drive mechanism; the rotor is filled with the packing material as described in any one of claims 1-7, the rotor is located inside the housing, the top center of the housing has a liquid inlet connected to the liquid distributor, the liquid distributor is located at the center of the packing material inside the rotor; the bottom of the housing has a liquid outlet; the drive mechanism is connected to the rotor and is used to drive the rotor to rotate; the sealing device is used to ensure the sealing performance of the supergravity rotation devolatilization device.

9. The supergravity rotational devouring device according to claim 8, characterized in that, The outer side of the housing is provided with a jacket for heating the supergravity rotation devouring device; the housing is also provided with a pressure relief port.

10. The supergravity rotational devouring device according to claim 8, characterized in that, The drive mechanism includes a rotating shaft and a motor; the upper end of the rotating shaft is fixedly connected to the rotor, and the lower end of the rotating shaft is connected to the motor through a bearing; the sealing device includes at least one of a shaft seal, an O-ring, and an oil seal.

11. A high-viscosity polymer devolatilization system, characterized in that, It includes a high-gravity rotary devolatilization device, a vacuum unit, and a feeding unit; the high-gravity rotary devolatilization device has a rotor at its center filled with the packing material as described in any one of claims 1-7; the feeding unit is connected to the liquid inlet of the high-gravity rotary devolatilization device, and the vacuum unit is connected to the liquid outlet of the high-gravity rotary devolatilization device.

12. The high-viscosity polymer devolatilization system according to claim 11, characterized in that, The vacuum unit includes: a vacuum pump, a piezoresistive vacuum gauge, a discharge liquid storage tank, a condenser, a gas-liquid separator, and an adsorption tank; the vacuum pump is a rotary vane vacuum pump; the discharge liquid storage tank has four ports at the top and a discharge port at the bottom; one port at the top of the discharge liquid storage tank is connected to the liquid outlet at the bottom of the supergravity rotary devolatilization device, the discharge liquid storage tank is connected to the condenser, and another port at the top of the discharge liquid storage tank is also connected to a connection port on the side wall of the shell of the supergravity rotary devolatilization device to maintain a constant vacuum level in the devolatilization system; the condenser is connected to the top of the gas-liquid separator, one side of the gas-liquid separator is connected to the top of the adsorption tank, and the bottom of the adsorption tank is connected to the vacuum pump; The adsorption tank is filled with 5A molecular sieves or activated carbon.

13. The high-viscosity polymer devolatilization system according to claim 11, characterized in that, The feeding unit includes: a melting tank, a raw material liquid storage tank, and a gear pump; the melting tank is used for melting the polymer, the top of the raw material liquid storage tank is provided with a feed inlet and a vent, and the bottom of the raw material liquid storage tank is provided with a discharge outlet; the feed inlet of the raw material liquid storage tank is connected to the melting tank, and the discharge outlet of the raw material liquid storage tank is connected to the gear pump; the gear pump is a gear metering pump suitable for conveying high-viscosity media; the gear pump is connected to the liquid inlet of the high-gravity rotary devolatilization device, and a flow meter is also provided between the gear pump and the high-gravity rotary devolatilization device.

14. A method for removing volatiles from polymers using ultragravity, characterized in that, Includes the following steps: (1) Add the polymer solution containing volatiles to the raw material storage tank; (2) Turn on the vacuum pump to bring the entire system into a vacuum state; (3) Activate the hypergravity rotation devouring device: turn on the motor and set the hypergravity factor; (4) Start the gear pump and inject the polymer solution into the gravity rotary devolatilization device through the inlet; (5) Determination of volatile content: After the polymer solution is treated by the supergravity rotary devolatilization device, a sample is taken from the outlet to detect the volatile content.

15. The method for removing volatiles from polymers using ultragravity according to claim 14, characterized in that, In step (2), the vacuum degree of the entire system is 0.08 to 0.095 MPa; In step (3), the hypergravity factor is set to 30-90; The temperature of the polymer solution is 25–160°C, and the mass content of volatile matter is 5%–20%; the flow rate of the polymer solution is 0.1–1.5 m / s.

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