CN115920428B - Device for devolatilization of polymer and devolatilization method of polyolefin elastomer - Google Patents
Device for devolatilization of polymer and devolatilization method of polyolefin elastomer Download PDFInfo
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Abstract
本发明公开了一种用于聚合物脱挥的装置及聚烯烃弹性体脱挥方法，该装置由多级脱挥器组成，每一级脱挥器入口设置有椭球台形进料分布器，前级脱挥器入口采用进料预热器进行加热，最后级脱挥器直接通入蒸汽进行加热，采用本发明的脱挥装置进行脱挥，物料成膜性好，得到的物料挥发分含量小，脱挥效率高。The invention discloses a device for devolatilization of polymer and a devolatilization method for polyolefin elastomer. The device is composed of a multi-stage devolatilizer. An ellipsoidal cone-shaped feed distributor is arranged at the inlet of each stage of the devolatilizer. A feed preheater is used to heat the inlet of the front stage devolatilizer. Steam is directly introduced into the last stage devolatilizer for heating. When the devolatilization device of the invention is used for devolatilization, the material has good film-forming property, the volatile content of the obtained material is small, and the devolatilization efficiency is high.
Description
Technical Field
The invention belongs to the technical field of high polymer material production and processing, relates to elastomer devolatilization production technology, and in particular relates to a polymer devolatilization device and a polyolefin elastomer devolatilization method.
Background
Most polymers at the outlet of the polymerization reactor contain low-relative-molecular-weight components such as monomers, solvents, water, byproducts and the like, and the content of the volatile components is generally 10-80 wt% according to different processes, so that the volatile components need to be further removed, thereby meeting the requirements of improving the performance, health and environment of the polymers, recycling the solvents and the monomers and the like. With the continuous increase of safety, environmental protection and health level, the requirements of different application fields on the VOC content in the polymer material are also continuously increasing, for example, the content of acrylonitrile in the food-grade ABS product is required to be lower than 5ppm.
The polyolefin elastomer is a random copolymer of metallocene catalyzed ethylene and alpha-olefin, has excellent weather resistance and chemical resistance, good compatibility with polyolefin, high elasticity of rubber and easy processability of plastic, and the obtained elasticity has lower cost, lighter weight, lower energy consumption and more environmental friendliness. The synthesis generally adopts a solution polymerization process. The polymer solid at the outlet of the reactor only accounts for 8-25wt% of the reaction mother liquor, the unreacted completely polymerized monomers in the mother liquor comprise ethylene, alpha-olefin and solvent, and then the slurry is conveyed into a devolatilizer after the reactor to remove the unreacted monomers and solvent. The structural design of the devolatilizer and the control of the process parameters are critical factors related to the VOC index in the final polyolefin elastomer product.
There are few patents currently published for devolatilization of polyolefin elastomers. In industry, widely used polymer devolatilization processes comprise a falling strip devolatilizer, an in-pipe falling film devolatilizer and the like, and the solvent and the monomer are removed by preheating the feed and vacuumizing the devolatilizer, so that the interface is continuously updated in the falling process of the polymer melt. In order to diffuse the volatiles as far as possible from the constantly updated interface to enhance devolatilization, it is common in the industry to maximize the preheating temperature and vacuum of the feed. However, according to the studies of Park and Suh et al, the rapid increase in temperature or decrease in pressure places the polymer solution in a thermodynamically unstable supersaturated state, and bubble nuclei are easily formed at the interface, so that the volatile components exist in the form of bubbles. The nucleation, growth and collapse process of bubbles becomes a control step in the devolatilization process. Only when the bubbles are finally broken, volatile components in the bubbles can be diffused out, so that the devolatilization effect of the devolatilizer is seriously affected in the foaming devolatilization process. Therefore, optimization is expected to be performed on the existing devolatilization equipment, the interface update of the melt is improved, and the rapid collapse of bubbles is realized, so that the devolatilization effect is improved.
Disclosure of Invention
The invention aims to provide a device for polymer devolatilization, which can update the melt interface quickly in the devolatilization process, quickly break bubbles and has high devolatilization efficiency.
The invention also aims to provide a polyolefin elastomer devolatilization method, which adopts a multistage (more than or equal to two stages) static devolatilization process, has high devolatilization efficiency and ensures that the residual volatile organic compounds of the product are less than 2000ppm.
To achieve the technical object, the present invention provides a devolatilization apparatus, comprising: the pre-stage devolatilizer comprises a feeding distributor, a preheater and a devolatilization tank, wherein the feeding distributor is fixed at the top of the preheater, the devolatilization tank is positioned below the preheater, the materials enter the preheater through the distributor to be heated, the devolatilization tank is positioned below the preheater and connected through a flange, a melt feeding pump is positioned at the bottom of the devolatilization tank, and the feeding distributor is provided with ellipsoidal holes;
The final-stage devolatilizer comprises a feeding distributor, a steam feeding pipe and a devolatilizing tank, wherein the feeding distributor is fixed at the top of the preheater, an elliptic table-shaped hole is formed in the feeding distribution plate, and the steam feeding pipe is arranged below the feeding distributor. According to different specific devolatilization processes, the front-stage devolatilizer can be connected in series with the last-stage devolatilizer after one-stage or multi-stage serial connection, and the front-stage devolatilizer sends materials to the top of the rear-stage devolatilizer through a melt pump through a pipeline.
In some preferred embodiments of the present invention, the ellipsoidal table shaped holes are uniformly distributed on the feed distributor in a regular triangle shape, the ellipsoidal table upper bottom ellipse is concentric with the lower bottom ellipse, and the upper bottom ellipse area is larger than the lower bottom, and the ellipsoidal table height is equal to the thickness of the feed distribution plate.
Preferably, the center distance between the upper bottom ellipses is 1-5 times of the major axis of the upper bottom ellipses.
Preferably, the elliptical long axis of the upper bottom of the elliptical table-shaped hole is 2-8 times of the elliptical long axis of the lower bottom, the elliptical long axis of the upper bottom is 20-40mm, and the elliptical short axis of the upper bottom and the lower bottom is 0.2-5 times of the length of the long axis
Preferably, the inlet of the steam feed pipe of the final-stage devolatilizer is provided with a circular ring pipe distributor, the outer diameter of the ring pipe distributor is equal to the diameter of the feeding distribution plate of the final-stage devolatilizer, and circular holes are uniformly formed in the ring pipe.
Preferably, the diameter of the round holes is 6-12mm, the center distances of any two adjacent round holes are equal, and the center distance is 3-10 times of the diameter of the round holes; preferably 3-8 times.
Preferably, the loop distributor is located 20-100mm below the feed distribution plate.
The invention also provides a devolatilization process of the polyolefin elastomer by adopting the devolatilization device, which comprises the following steps:
s1: delivering the outlet material of the polyolefin elastomer reactor to a pre-devolatilizer for devolatilization;
S2, after the devolatilization in the step S1 is completed, conveying the devolatilized product to a final-stage devolatilizer for devolatilization;
s3: and (3) discharging after the devolatilization in the step S2 is completed.
Further, the step S1 further includes the following steps:
A1: the material enters a feeding distributor at the top of a pre-stage devolatilizer, is uniformly distributed by the distributor material, and enters a heat exchange tube of a preheater;
A2: the polymer melt is evaporated in a falling film in a heat exchange tube, and a heating medium is arranged outside the tube;
A3: the material flows out of the preheater, enters a bottom devolatilization tank, and is flash vaporized in the tank.
Further, the step S2 further includes the following steps:
B1: the material at the outlet of the front-stage devolatilizer is pumped to the final-stage devolatilizer, and the material is uniformly distributed through a feeding distributor at the top and then enters a devolatilization tank in a falling strip shape;
B2: the steam is uniformly dispersed into the gas phase space in the tank through the annular pipe distributor, and meanwhile, the falling strips are heated and stripped.
B3: the second-stage devolatilizer is provided with a pressure control loop for adjusting the steam supplementing and the pumping speed of the vacuum pump, and maintains different operating pressures according to different feed temperatures and solid contents; the steam enters the devolatilizer through the loop distributor to be instantaneously expanded, and the strip-shaped material is contacted with the steam to generate superheat degree, so that volatile components are rapidly removed under the high vacuum condition.
In some preferred embodiments of the invention, the feed is preferably a reactor outlet polyolefin elastomer solution, wherein the polymer solids content is 8-25wt%, the volatiles content is 75% -92wt%, and the feed temperature is 140-160 ℃.
Preferably, the preheater is a single-tube-pass single-shell-pass shell-and-tube heat exchanger, the shell-pass heating medium adopts hot oil, the inlet temperature of the hot oil is 270-290 ℃, and the outlet temperature of the tube-pass material is 260-280 ℃.
Preferably, the in-tube medium is a polyolefin elastomer melt and the out-tube heating medium is steam or hot oil or the like.
Preferably, the operation temperature of the front-stage devolatilizer is 200-240 ℃, the operation pressure is 0.15-0.35MpaG, and the apex angle of the bottom cone of the devolatilizer is 75-90 degrees.
Depending on the number of series stages (typically no more than four stages) and the ratio of solvent removal per stage, the temperature drop of the devolatilizer after the subsequent stage of preheating is typically within 10 ℃ in terms of the operating temperature of the devolatilizer, i.e., if the operating temperature of the previous stage of devolatilizer is 220 ℃, the subsequent stage is preheated to 240 ℃ by the preheater and the operating temperature of the subsequent stage of devolatilizer is between 230 and 240 ℃. Preferably, the preheating temperature of the final-stage devolatilizer is 240-260 ℃, and the operating temperature of the intermediate-stage devolatilizer is 230-250 ℃.
Depending on the number of series stages (typically no more than four stages) and the ratio of solvent removal per stage, the operating pressure of the devolatilizer at the subsequent stage is typically lower than that at the previous stage, typical of the four-stage devolatilizer series operation: the operating pressure of the first-stage devolatilizer is 0.15-0.35 MpaG, the operating pressure of the second stage is 0-0.1 MpaG, the operating pressure of the third stage is 10-100 kpaA, and the operating pressure of the last stage is less than 10kpaA.
Preferably, the volatile component of the material leaving the pre-devolatilizer is 5-15 wt% and the temperature is 200-240 ℃.
Preferably, the temperature of the steam of the final-stage devolatilizer is 240-260 ℃ and the pressure is 3-4MpaG;
preferably, the pressure of the final devolatilizer is 0.1-2kpA, and the apex angle of the bottom cone of the devolatilizer is 75-90 degrees.
Preferably, the volatile content of the final devolatilizer outlet material is less than 2000ppm.
The beneficial effects of the invention are as follows:
1. Compared with the uniform round or grid-slit-shaped open-pore elements in the traditional falling-strand or falling-film static devolatilizer, the device provided by the invention has the advantages that the feeding distributor is provided with the oval table-shaped open-pore elements with small top and bottom, and the design has two advantages: on one hand, when the huge pressure on two sides of the distributor is reduced, materials enter the holes of the elliptical table, the elliptical area on the top is large and is distributed in a regular triangle shape, so that the materials are convenient to uniformly disperse, the aperture is smaller and smaller in the downward process along the holes, the flow speed is faster and faster, the surface of a melt is facilitated to be updated, and finally the melt flows out through the small holes on the bottom to be in a fine falling strip shape, and the removal of volatile matters in the falling process is facilitated; on the other hand, under high vacuum and high superheat, bubble nuclei are extremely easy to form on the surface of the melt, but because the open-pore element is elliptical, the bubble nuclei are limited in growth and are not easy to grow up in the short axis direction, the included angle between the inner surface of the hole and the horizontal direction is larger than the equilibrium contact angle of the melt, the bubbles generate a yielding phenomenon to start sliding, and when the melt flows out of the open-pore element, the bubbles are rapidly separated from the surface of the melt.
2. On one hand, the solid content of the melt at the inlet of the final stage reaches 95-99wt percent, compared with the viscosity at the inlet of the first stage, the viscosity of the melt is obviously increased, the melt is subjected to laminar flow in a tube by adopting a traditional tube type heat exchanger, the heat transfer coefficient is very small, the heat exchange effect is poor, and the melt is subjected to direct contact heating by adopting steam, so that the heat transfer efficiency is high, and the investment of expensive high-viscosity heat exchanger equipment is saved; on the other hand, when the high-pressure steam enters the devolatilizer through the annular pipe distribution small holes, the flow speed is very high, the steam volume is rapidly expanded due to high vacuum, the steam is wrapped when falling down, and the volatile concentration in the gas phase is diluted, so that huge concentration gradient exists in the volatile melt and the gas phase space, and the removal efficiency of the volatile is remarkably improved. Meanwhile, the continuous blowing of steam inhibits bubble nucleation on the surface of the melt and accelerates the separation of bubbles from the surface of the melt.
By adopting the process, the heat transfer effect is greatly enhanced, the film forming area is increased, the surface renewal of a liquid film is promoted, the devolatilization efficiency is improved, and the volatile matters in the polyolefin elastomer can be removed to below 2000ppm through two-stage static devolatilization. And meanwhile, the melt is heated more uniformly, so that the phenomena of yellowing and black spots of materials are avoided due to high local temperature.
Drawings
FIG. 1 is a schematic flow diagram of a two-stage polyolefin elastomer devolatilization process of the present invention;
FIG. 2 is a schematic structural view of a front-stage devolatilizer of the present invention;
FIG. 3 is a schematic view showing the structure of a final devolatilizer of the present invention;
FIG. 4 is a schematic view of devolatilizer inlet distributor openings;
fig. 5 is a schematic view of a steam feed loop distributor.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and examples:
As shown in fig. 1, in the embodiment of the present invention, a devolatilization system is used, which includes a primary devolatilizer D01 and a primary devolatilized melt feed pump P01; a secondary devolatilizer D02 and a secondary melt pump P02. The top of the primary devolatilization preheater E01 is provided with a feeding distributor, the secondary devolatilization device D02 is also internally provided with a material distributor, and polyolefin elastomer materials flow along the direction from top to bottom.
As shown in fig. 2 and 4, the primary devolatilizer D01 comprises a primary feed distributor 1, a preheater 2 and a primary devolatilizing tank 3, the primary feed distributor 1 is fixed at the top of the preheater 2, the primary devolatilizing tank 3 is located below the preheater and connected through a flange, the primary melt feed pump P01 is located at the bottom of the devolatilizing tank, ellipsoidal table-shaped holes are formed in the primary feed distributor 1, the ellipsoidal table-shaped holes are uniformly distributed in a regular triangle shape on the feed distribution plate, the ellipse of the upper bottom of the ellipsoidal table is concentric with that of the lower bottom, the elliptical area of the upper bottom is larger than that of the lower bottom, and the ellipsoidal table height is equal to the thickness of the feed distributor.
As shown in fig. 3 and 4, the secondary devolatilizer D02 comprises a secondary feed distributor 4, a steam feed pipe 2 and a secondary devolatilizing tank 6, wherein the secondary feed distributor 4 is fixed at the top of the devolatilizer, the secondary feed distributor 4 is provided with an elliptic table-shaped hole, and the steam feed pipe 2 is arranged below the feed distributor. As shown in fig. 5, the inlet of the steam feed pipe of the secondary devolatilizer is provided with a circular loop distributor.
Example 1:
In this example, the flow rate of the polyolefin elastomer solution entering the first devolatilizer was 200kg/h, the solid content was 8wt%, and the temperature was 140 ℃. The primary preheater is heated by hot oil at 270 ℃, the temperature of polyolefin elastomer solution at the outlet of the primary preheater is 260 ℃, the operating temperature of the primary devolatilizer is 240 ℃, and the operating pressure is 0.35MpaG.
The feeding distributor of the primary devolatilizer is provided with 150 holes, the major axis of the ellipse at the top of the elliptical table is 20mm, the minor axis is 10mm, the center distance is 100mm, the major axis of the ellipse at the bottom is 5mm, the minor axis is 2.5mm, and the bottom cone angle of the primary devolatilizer is 75 degrees.
The polyolefin elastomer solution at the inlet of the secondary devolatilizer had a solids content of 95wt% (i.e., a volatile content of 5 wt%) and a feed temperature of 220 ℃. The secondary devolatilizer was heated by passing 3MpaG at 240 ℃. The operating temperature of the secondary devolatilizer was 235℃and the operating pressure was 2kpaA ℃and the outlet polyolefin elastomer melt temperature was 235℃and the VOC content of the outlet melt was 1925ppm.
The feeding distributor of the secondary devolatilizer is provided with 150 holes, the major axis of the ellipse at the top of the elliptical table is 16mm, the minor axis is 8mm, the center distance is 40mm, the major axis of the ellipse at the bottom is 4mm, the minor axis is 2mm, and the apex angle of the bottom cone of the devolatilizer is 75 degrees.
The number of round holes formed in the steam feeding circular pipe is 40, the diameter is 6mm, and the center distance between two adjacent round holes is 18mm.
Example 2:
In this example, the flow rate of the polyolefin elastomer solution entering the first devolatilizer was 300kg/h, the solid content was 15wt%, and the temperature was 150 ℃. The primary preheater is heated by hot oil at 285 ℃, the temperature of the polyolefin elastomer solution at the outlet of the primary preheater is 270 ℃, the operating temperature of the primary devolatilizer is 240 ℃, and the operating pressure is 0.25MpaG.
The feeding distributor of the primary devolatilizer is provided with 220 holes, the major axis of the ellipse at the top of the elliptical table is 24mm, the minor axis is 7.2mm, the center distance is 72mm, the major axis of the ellipse at the bottom is 4mm, the minor axis is 1.6mm, and the bottom cone angle of the primary devolatilizer is 80 degrees.
The polyolefin elastomer solution at the inlet of the secondary devolatilizer had a solids content of 90wt% (i.e., 10wt% of volatiles) and a feed temperature of 240 ℃. The secondary devolatilizer was heated by passing 3.5MpaG steam at 245 ℃. The operating temperature of the secondary devolatilizer was 243℃and the operating pressure was 0.5kpaA, the temperature of the outlet polyolefin elastomer melt was 243℃and the VOC content of the outlet melt was 1682ppm.
The feeding distributor of the secondary devolatilizer is provided with 150 holes, the major axis of the ellipse at the top of the elliptical table is 16mm, the minor axis is 8mm, the center distance is 32mm, the major axis of the ellipse at the bottom is 4mm, the minor axis is 1.6mm, and the bottom cone angle of the primary devolatilizer is 80 degrees.
The number of round holes formed in the steam feeding circular pipe is 34, the diameter is 8mm, and the center distance between two adjacent round holes is 40mm.
Example 3:
In this example, the flow rate of the polyolefin elastomer solution entering the first devolatilizer was 600kg/h, the solid content was 25wt%, and the temperature was 160 ℃. The primary preheater is heated by hot oil at 270 ℃, the temperature of polyolefin elastomer solution at the outlet of the primary preheater is 240 ℃, the operating temperature of the primary devolatilizer is 200 ℃, and the operating pressure is 0.35MpaG.
The feeding distributor of the primary devolatilizer is provided with 310 holes, the major axis of the ellipse at the top of the elliptical table is 40mm, the minor axis is 8mm, the center distance is 40mm, the major axis of the ellipse at the bottom is 5mm, the minor axis is 1mm, and the bottom cone angle of the primary devolatilizer is 90 degrees.
The polyolefin elastomer solution at the inlet of the secondary devolatilizer had a solids content of 85wt% (i.e., a volatile content of 15 wt%) and a feed temperature of 200 ℃. The secondary devolatilizer was heated by passing 4MpaG at 260 ℃. The operating temperature of the secondary devolatilizer was 250℃and the operating pressure was 0.1kpaA, the temperature of the outlet polyolefin elastomer melt reached 250℃and the VOC content of the outlet melt was 1714ppm.
The feeding distributor of the secondary devolatilizer is provided with 310 holes, the major axis of the ellipse at the top of the elliptical table is 12mm, the minor axis is 6mm, the center distance is 24mm, the major axis of the ellipse at the bottom is 3mm, the minor axis is 1.5mm, and the bottom cone angle of the primary devolatilizer is 90 degrees.
The number of round holes formed in the steam feeding circular pipe is 20, the diameter is 12mm, and the center distance between two adjacent round holes is 96mm.
Comparative example 1:
In this example, the flow rate of the polyolefin elastomer solution entering the first devolatilizer was 300kg/h, the solid content was 15wt%, and the temperature was 150 ℃. The primary preheater is heated by hot oil at 285 ℃, the temperature of the polyolefin elastomer solution at the outlet of the primary preheater is 270 ℃, the operating temperature of the primary devolatilizer is 224 ℃, and the operating pressure is 0.25MpaG.
The feeding distributor of the primary devolatilizer is provided with 220 holes,Is arranged at a center distance of 72mm.
The polyolefin elastomer solution at the inlet of the secondary devolatilizer had a solids content of 80wt% (i.e., a volatile content of 20 wt%) and a feed temperature of 224 ℃. The secondary devolatilizer was heated by passing 3.5MpaG steam at 245 ℃. The operating temperature of the secondary devolatilizer was 232℃and the operating pressure was 0.5kpaA, the temperature of the outlet polyolefin elastomer melt reached 232℃and the VOC content of the outlet melt was 9523ppm.
The feeding distributor of the secondary devolatilizer is provided with 150 holes, the major axis of the ellipse at the top of the elliptical table is 16mm, the minor axis is 8mm, the center distance is 32mm, the major axis of the ellipse at the bottom is 4mm, the minor axis is 1.6mm, and the apex angle of the bottom cone of the devolatilizer is 80 degrees.
The number of round holes formed in the steam feeding circular pipe is 34, the diameter is 8mm, and the center distance between two adjacent round holes is 40mm.
Comparative example 2:
In this example, the flow rate of the polyolefin elastomer solution entering the first devolatilizer was 300kg/h, the solid content was 15wt%, and the temperature was 150 ℃. The primary preheater is heated by hot oil at 285 ℃, the temperature of the polyolefin elastomer solution at the outlet of the primary preheater is 270 ℃, the operating temperature of the primary devolatilizer is 240 ℃, and the operating pressure is 0.25MpaG.
The feeding distributor of the primary devolatilizer is provided with 220 holes, the major axis of the ellipse at the top of the elliptical table is 24mm, the minor axis is 7.2mm, the center distance is 72mm, the major axis of the ellipse at the bottom is 4mm, the minor axis is 1.6mm, and the apex angle of the bottom cone of the devolatilizer is 80 degrees.
The polyolefin elastomer solution at the inlet of the secondary devolatilizer had a solids content of 90wt% (i.e., 10wt% of volatiles) and a feed temperature of 240 ℃.
The feeding distributor of the secondary devolatilizer is provided with 150 holes,Is arranged at a hole pitch of 32mm. The bottom of the secondary distributor is a common shell and tube heat exchanger, materials are moved in the heat exchange tube, hot oil at 245 ℃ is introduced outside the tube, the outlet temperature of the heat exchanger is 243 ℃, the operating pressure in the devolatilization tank is 0.5kpaA, the temperature of the polyolefin elastomer melt at the outlet reaches 238 ℃, the VOC content in the melt reaches 1.5 weight percent, a large number of primary bubbles are arranged in the melt, a large number of tiny secondary bubbles are arranged on the inner wall of the primary bubbles, the flow rate of a discharged material pump of the melt at the bottom is obviously lower than the normal flow rate, and the liquid level control of a melt pool at the taper section of the devolatilization tank is unstable.
Claims (17)
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| DE10333577A1 (en) * | 2003-07-24 | 2005-02-24 | Bayer Technology Services Gmbh | Method and apparatus for removing volatile substances from highly viscous media |
| CN208229449U (en) * | 2018-04-04 | 2018-12-14 | 星辉化学股份有限公司 | High viscosity fluid devolatilization staged cloth flow tube |
| CN108654124B (en) * | 2018-05-31 | 2020-11-24 | 万华化学集团股份有限公司 | Device and method for removing volatile organic compounds in emulsion |
| CN112724296A (en) * | 2020-12-28 | 2021-04-30 | 江苏可立特工程设计研究有限公司 | Transparent polystyrene with capacity of more than 5 ten thousand tons and production equipment and process thereof |
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| CN101422717A (en) * | 2008-11-21 | 2009-05-06 | 中国蓝星（集团）股份有限公司 | Gas liquid mixed feeding distributor and polyphenylene oxide reaction device using the same |
| CN104086349A (en) * | 2013-04-01 | 2014-10-08 | 中国石油化工股份有限公司 | Method for oligomerization production of alpha olefin from ethylene |
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