CN216935949U - Polymerization reaction device - Google Patents
Polymerization reaction device Download PDFInfo
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- CN216935949U CN216935949U CN202220054266.4U CN202220054266U CN216935949U CN 216935949 U CN216935949 U CN 216935949U CN 202220054266 U CN202220054266 U CN 202220054266U CN 216935949 U CN216935949 U CN 216935949U
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Abstract
The present invention relates to a polymerization reaction apparatus comprising: the polymerization reactor is connected with the heating device to provide a temperature environment required by polymerization reaction; the first feeding assembly is arranged on the polymerization reactor to convey materials to be reacted into the polymerization reactor, and the materials to be reacted form a pressurized environment higher than atmospheric pressure in the polymerization reactor; a second feed assembly comprising: the system comprises at least one feeding tank, at least one feeding tank and a control device, wherein the feeding tanks are sequentially communicated, one of the at least one feeding tank is detachably arranged on a polymerization reactor so as to convey a catalyst and a monomer into the polymerization reactor, and the catalyst, the monomer and a material are added into the polymerization reactor in a pressurized environment; a vacuum assembly in communication with the polymerization reactor, the vacuum assembly configured to create a vacuum environment within the polymerization reactor prior to input of a material to be reacted into the polymerization reactor; and an isobaric device detachably connected between the second feeding assembly and the polymerization reactor to maintain equal pressure in the feeding tank and the polymerization reactor.
Description
Technical Field
The utility model relates to the technical field of macromolecules and chemical engineering, in particular to a polymerization reaction device.
Background
Polyethylene is the most widely used artificial and synthetic resin, and has the advantages of low price, excellent performance and easy processing and forming. Polyethylene is polymerized from ethylene as a monomer, or is copolymerized from ethylene and a small amount of alpha-olefin monomer.
In general, polyethylene is prepared by the copolymerization of ethylene monomer or ethylene and olefin monomer catalyzed by a catalyst, and is usually polymerized in a gas-liquid phase combination. In the traditional process, a solvent and a comonomer are added into a reactor for preheating, a main catalyst and a cocatalyst are premixed and then added in an injection mode, and then the premixed main catalyst and the cocatalyst are introduced into an ethylene reactor with certain pressure. The process is simple and efficient, but has disadvantages in that the needle inevitably comes into contact with air during injection, which may cause catalyst deactivation, and olefin polymerization at high temperature (more than 150 ℃) and high pressure (more than 10 atm) cannot be performed. Therefore, there is a need to design a catalyst and monomer feeding assembly, which can be added into an olefin polymerization reactor in a strict anhydrous and oxygen-free environment to activate the catalyst in an environment where a certain ethylene pressure exists, so as to avoid catalyst deactivation, and at the same time, the catalyst and monomer feeding assembly can be combined according to different requirements of products to produce different types of products, so that a flexible combination mode is provided.
SUMMERY OF THE UTILITY MODEL
In view of the above, the present invention provides a polymerization apparatus.
In one aspect of the present invention, there is provided a polymerization reaction apparatus comprising: the polymerization reactor is connected with the heating device to provide a temperature environment required by polymerization reaction; the first feeding assembly is arranged on the polymerization reactor to convey materials to be reacted into the polymerization reactor, and the materials to be reacted form a pressurized environment higher than atmospheric pressure in the polymerization reactor; a second feed assembly comprising: the system comprises at least one feeding tank, at least one feeding tank and a control device, wherein the feeding tanks are sequentially communicated, one of the at least one feeding tank is detachably arranged on a polymerization reactor so as to convey a catalyst and a monomer into the polymerization reactor, and the catalyst, the monomer and a material are added into the polymerization reactor in a pressurized environment; a vacuum assembly in communication with the polymerization reactor, the vacuum assembly configured to create a vacuum environment within the polymerization reactor prior to input of a material to be reacted into the polymerization reactor; and an isobaric device detachably connected between the second feeding assembly and the polymerization reactor to maintain equal pressure in the feeding tank and the polymerization reactor.
According to an embodiment of the utility model, the second feeding assembly further comprises: and the plurality of feeding valves are respectively arranged at the input end and the output end of the second feeding assembly and between the two adjacent feeding tanks.
According to an embodiment of the utility model, the second feeding assembly further comprises: the first end of the isobaric device is detachably communicated with the feeding tank through one port of the first three-way valve.
According to an embodiment of the present invention, the vacuum assembly includes a second three-way valve having a first port in communication with the polymerization reactor, a second port in communication with the vacuum assembly, and a third port in communication with the second end of the isobaric device.
According to an embodiment of the utility model, the first feeding assembly comprises: a conduit having one end in communication with the polymerization reactor; the gas cylinder is communicated with the other end of the guide pipe and stores olefin monomer gas; and the purification device is communicated with the gas cylinder to provide the olefin monomer gas with qualified impurity content.
According to an embodiment of the present invention, the polymerization reactor is connected to the first feeding assembly by a quick-connect coupling.
According to the embodiment of the utility model, the method further comprises the following steps: the fixing part is arranged on the polymerization reactor so as to install the polymerization reactor on the support frame.
According to an embodiment of the present invention, further comprising: and the pressure gauge is arranged on the polymerization reactor and used for detecting the pressure inside the polymerization reactor.
According to an embodiment of the present invention, further comprising: a motor mounted on the polymerization reactor; and the stirring paddle is arranged in the polymerization reactor and is driven by the motor to stir the materials in the polymerization reactor.
According to the embodiment of the utility model, the method further comprises the following steps: the pressure sensor is arranged on a pipeline communicated with the polymerization reactor and used for detecting and transmitting the pressure inside the polymerization reactor; and the regulating valve is arranged on a pipeline communicated with the polymerization reactor, sets preset pressure, and regulates the internal pressure of the polymerization reactor according to the pressure in the polymerization reactor.
In the polymerization reaction device, the second feeding assembly for conveying the catalyst and the monomer is detachably connected with the polymerization reactor, so that the second feeding assembly can be detached from the polymerization reactor, the catalyst and the monomer are premixed in a water-free and oxygen-free environment, and then the second feeding assembly is connected with the polymerization reactor and conveys the catalyst and the monomer into the polymerization reactor, so that the catalyst can be activated in an environment with certain ethylene pressure, and the catalyst can be prevented from being deactivated.
Drawings
FIG. 1 is a schematic front view of a polymerization reaction apparatus according to an embodiment of the present invention;
FIG. 2 is a physical diagram of a polymerization reaction apparatus according to an embodiment of the present invention; and
FIG. 3 is a material flow diagram of an embodiment of the present invention.
Description of the reference numerals
1 polymerization reactor
2 first feeding assembly
21 catheter
3 second feeding assembly
31 feeding tank
32 feed valve
33 first three-way valve
4 vacuum assembly
41 second three-way valve
5 equipressure device
6 fixed part
7 pressure gauge
8 electric machine
9 pressure sensor
10 regulating valve
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
In the traditional process for preparing polyethylene, a solvent and a comonomer are added into a reactor for preheating, a main catalyst and a cocatalyst are premixed and then added in an injection mode, and then the premixed main catalyst and the cocatalyst are introduced into an ethylene reactor with certain pressure. The process is simple and efficient, but has disadvantages in that the needle inevitably comes into contact with air during injection, which may cause catalyst deactivation, and olefin polymerization at high temperature (more than 150 ℃) and high pressure (more than 10 atm) cannot be performed.
To this end, according to the general inventive concept of one aspect of the present invention, there is provided a polymerization reaction apparatus including: the polymerization reactor is connected with the heating device to provide a temperature environment required by polymerization reaction; the first feeding assembly is arranged on the polymerization reactor to convey materials to be reacted into the polymerization reactor, and the materials to be reacted form a pressurized environment higher than atmospheric pressure in the polymerization reactor; a second feed assembly comprising: the system comprises at least one feeding tank, at least one feeding tank and a control device, wherein the feeding tanks are sequentially communicated, one of the at least one feeding tank is detachably arranged on a polymerization reactor so as to convey a catalyst and a monomer into the polymerization reactor, and the catalyst, the monomer and a material are added into the polymerization reactor in a pressurized environment; a vacuum assembly in communication with the polymerization reactor, the vacuum assembly configured to create a vacuum environment within the polymerization reactor prior to input of a material to be reacted into the polymerization reactor; and an isobaric device detachably coupled between the second feeding assembly and the polymerization reactor to maintain equal pressures in the feed tank and the polymerization reactor.
In the polymerization reaction device, the second feeding assembly used for conveying the catalyst and the monomer is detachably connected with the polymerization reactor, the second feeding assembly can be detached from the polymerization reactor, the catalyst and the monomer are premixed in a water-free and oxygen-free environment, and then the second feeding assembly is connected with the polymerization reactor and conveys the catalyst and the monomer to the polymerization reactor, so that the catalyst can be activated in an environment with certain ethylene pressure, the catalyst is prevented from being deactivated, and meanwhile, the combination of the catalyst and the monomer can be carried out according to different requirements of products, and a flexible combination mode is provided to produce different types of products.
The technical solution of the present invention will be described in detail below with reference to specific examples. It should be noted that the following specific examples are only for illustration and are not intended to limit the utility model.
FIG. 1 is a schematic front view of a polymerization reaction apparatus according to an embodiment of the present invention; FIG. 2 is a schematic view of a polymerization reaction apparatus according to an embodiment of the present invention.
As shown in fig. 1 and 2, the polymerization reaction apparatus of the present invention comprises: a polymerization reactor 1, a first feed assembly 2, a second feed assembly 3, a vacuum assembly 4, and an isobaric device 5. Wherein, the polymerization reactor 1 is connected with a heating device and is used for providing a high-temperature environment required by polymerization reaction; the first feeding assembly 2 is arranged on the polymerization reactor 1 and used for conveying materials to be reacted into the polymerization reactor 1, and the materials to be reacted form a pressurized environment higher than atmospheric pressure in the polymerization reactor 1; the second feed assembly includes: at least one feeding tank 31 which is communicated in sequence, wherein one of the at least one feeding tank 31 is detachably arranged on the polymerization reactor 1 so as to convey a catalyst and a monomer into the polymerization reactor 1, and the catalyst, the monomer and a material to be reacted are added into the polymerization reactor 1 in a pressurized environment for polymerization reaction; the vacuum component 4 is communicated with the polymerization reactor 1, and the vacuum component 4 is arranged to form a vacuum environment in the polymerization reactor 1 before the materials to be reacted, the catalyst and the monomers are input into the polymerization reactor 1; an isobaric device 5 is removably connected between the second feeding assembly 3 and the polymerization reactor 1 to maintain equal pressure inside the feeding tank 31 and the polymerization reactor 1. The second feeding assembly 3 for conveying the catalyst and the monomer is detachably connected with the polymerization reactor 1, the second feeding assembly 3 can be detached from the polymerization reactor 1, the catalyst and the monomer are premixed and then added into the olefin polymerization reactor 1 in the anhydrous and oxygen-free environment of the feeding tank 31 of the second feeding assembly 3, the catalyst is activated in the environment with certain ethylene pressure, and the catalyst is prevented from being deactivated.
According to the embodiment of the present invention, the polymerization reactor 1, the feed tank 31 and the isobaric device 5 are made of 316L stainless steel, and the polymerization reaction device can endure a high temperature of up to 200 ℃ and a high pressure of 50atm, and is suitable for the production of olefin homopolymers and copolymers, such as olefin homopolymers, ultrahigh molecular weight polyolefins, polar olefin copolymers, and the like.
According to the embodiment of the present invention, the polymerization reactor 1 is communicated with the second feeding module 3 by screw connection, so that each module can be freely connected and separated with the polymerization reactor 1. It will be appreciated that where the second feed assembly 3 is separate from the combined reactor 1, the interior of the second feed assembly 3 and the combined reactor 1 each form a separate enclosed environment.
According to an embodiment of the present invention, a plurality of feed tanks 31 can be provided in the second feeding assembly 3 to meet different polymerization requirements, and two feed tanks 31 are preferred in this embodiment.
According to an embodiment of the present invention, one of the charging tanks 31 stores a main catalyst and an optional modifier, wherein the main catalyst is solid particles and the modifier is liquid, and is finally prepared into slurry; another one of the feed tanks 31 stores the cocatalyst in solid particles and optionally the olefin monomer in liquid form, which is eventually made into a slurry.
According to an embodiment of the present invention, the second feeding assembly 3 further comprises a plurality of feeding valves 32 respectively disposed between the input end and the output end of the second feeding assembly 3 and two adjacent feeding tanks 31 for regulating the feeding of the materials into the polymerization reactor 1.
According to the embodiment of the utility model, before polymerization, the second feeding assembly 3 is separated from the polymerization reactor 1, the main catalyst, the cocatalyst and the comonomer are respectively added into the feeding tank 31 in the second feeding assembly 3 in a glove box with nitrogen or inert atmosphere, the material flow is regulated to the polymerization reactor 1 through the feeding valve 32, the whole process realizes feeding without injection in a water-free and oxygen-free environment, and the main catalyst and the cocatalyst are mixed under high temperature and high ethylene pressure, so that the catalyst deactivation is avoided.
According to an embodiment of the utility model, the second feeding assembly 3 further comprises: a first three-way valve 33 is provided at the input of the second feed assembly 3, and a first end of the isobaric device 5 is detachably connected to the feed tank 31 through a port of the first three-way valve 33.
According to an embodiment of the present invention, the vacuum assembly 4 comprises a second three-way valve 41, a first port of the second three-way valve 41 being in communication with the polymerization reactor 1, a second port being in communication with the vacuum assembly 4, and a third port being in communication with a second end of the isobaric device 5.
According to an embodiment of the utility model, the first feeding assembly 2 comprises: a conduit 21, one end of the conduit 21 communicating with the polymerization reactor 1; a gas cylinder communicating with the other end of the conduit to store an olefin monomer gas; and the purification device is communicated with the gas cylinder to provide the olefin monomer gas with qualified impurity content.
According to an embodiment of the utility model, the olefin monomer is a gas comprising any one of ethylene and propylene.
According to an embodiment of the present invention, the first feeding assembly 2 is equipped with a gas metering pump for metering the amount of material entering the polymerization reactor 1.
According to an embodiment of the present invention, the purification apparatus comprises at least one of a dehydration unit (for example, dehydration using a molecular sieve), a deoxidation unit (for example, deoxidation using a deoxidizer), a desulfurization unit (for example, desulfurization using a desulfurizing agent), a carbon monoxide removal unit, and a carbon dioxide removal unit for supplying the polymerization reactor 1 with an olefin monomer gas having an acceptable impurity content.
According to an embodiment of the present invention, the polymerization reactor 1 and the first feeding module 2 are connected by a quick coupling, so that each module can be freely connected and separated from the polymerization reactor 1.
According to an embodiment of the present invention, the polymerization reaction apparatus further comprises: the fixing part 6 is provided on the polymerization reactor 1 to mount the polymerization reactor 1 on a support frame (e.g., a table).
According to an embodiment of the present invention, the polymerization reaction apparatus further comprises: and a pressure gauge 7 disposed on the polymerization reactor 1 to detect the pressure inside the polymerization reactor 1.
According to an embodiment of the present invention, the polymerization reaction apparatus further comprises: a motor 8 installed on the polymerization reactor 1; and the stirring paddle is arranged in the polymerization reactor 1 and is driven by a motor to stir the materials in the polymerization reactor 1 so as to uniformly mix the reaction materials, the catalyst and the comonomer and fully react.
According to an embodiment of the present invention, the polymerization reaction apparatus further comprises: the pressure sensor 9 is arranged on a pipeline communicated with the polymerization reactor 1, is used for detecting and transmitting the pressure inside the polymerization reactor 1, and is connected with a computer terminal; and a control valve 10 which is provided in a pipe communicating with the polymerization reactor 1 and controls the pressure inside the polymerization reactor 1 according to the pressure inside the polymerization reactor 1.
According to the embodiment of the present invention, the charging valve 32 and the isobaric device 5 are ball valves made of 316L stainless steel, and satisfy the use range of up to 50atm and 200 ℃.
According to the embodiment of the utility model, the preset pressure of the regulating valve 10 is 6MPa, and when the preset pressure is exceeded, the regulating valve 10 can be opened to release gas, so that the overpressure protection effect on the polymerization reactor 1 is realized.
FIG. 3 is a material flow diagram of an embodiment of the present invention.
As shown in fig. 3, the material gas to be reacted in the first feeding assembly 2 is stored in a gas cylinder, passes through a purification device, and enters the polymerization reactor 1 through a conduit 21; meanwhile, in the second feeding assembly 3, the catalyst and the monomer are stored in the feeding tank 31, and are mixed and then enter the polymerization reactor 1 having high temperature and high pressure to perform polymerization reaction.
Example 1
The present invention will be further illustrated with reference to specific examples and the polymerization apparatus shown in FIG. 1.
This example is the preparation of an ethylene-octene copolymer.
First, the catalyst and octene monomer are loaded. Separating the second feeding assembly 3 from the polymerization reactor 1, and evacuating the interior of the combined reactor 1 to a vacuum environment by means of a vacuum assembly; thereafter, the second independent feeding unit 3 separated from the polymerization reactor 1 is transferred to a glove box, the main catalyst and the regulator are added to the upper feeding tank 31, the cocatalyst and the monomer are added to the lower feeding tank 31 under a nitrogen or inert gas anhydrous and oxygen-free atmosphere, and then all the feeding valves 32 and the isobaric device 5 are closed; at the same time, the first feeding assembly 2 is used to feed materials to be reacted, such as olefin monomer gas, into the combined reactor 1, so that a pressurized environment higher than atmospheric pressure is formed inside the polymerization reactor 1.
Next, gas-liquid phase ethylene-octene copolymerization. Connecting a second feeding assembly 3 filled with catalyst and monomer with the high-temperature high-pressure polymerization reactor 1, controlling the reaction temperature at 150 ℃ and the reaction pressure at 20atm, opening an isobaric device 5 and a part of feeding valves, making the liquid in two feeding tanks 31 flow into the polymerization reactor by using the isobaric titration principle, mixing and activating the main catalyst and the cocatalyst under the ethylene pressure of 20atm, and carrying out the copolymerization reaction of ethylene and octene.
And finally, after the polymerization is finished, the ethylene-octene copolymer product is obtained by subsequent collection and drying. The ethylene-octene copolymer obtained had a melting point of 99.33 ℃ as determined by DSC measurement, while having a molecular weight distribution of 4.2 as determined by GPC measurement.
According to the polymerization reaction device of the embodiment of the utility model, the second feeding assembly for conveying the catalyst and the monomer is detachably connected with the polymerization reactor, so that the second feeding assembly can be detached from the polymerization reactor, the catalyst and the monomer are premixed in a water-free and oxygen-free environment, then the polymerization reactor is connected with the polymerization reactor, and the catalyst and the monomer are conveyed into the polymerization reactor, therefore, the catalyst can be activated in an environment with certain ethylene pressure, the catalyst is prevented from being deactivated, and meanwhile, the combination of the catalyst and the monomer can be carried out according to different requirements of products, so that a flexible combination mode is provided, and different types of products can be produced.
It should also be noted that directional terms, such as "upper", "lower", "front", "rear", "left", "right", etc., used in the embodiments are only directions referring to the drawings, and are not intended to limit the scope of the present invention. Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present invention.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate the contents of the embodiments of the present invention. Furthermore, the word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements.
Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the utility model, various features of the utility model are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the utility model and aiding in the understanding of one or more of the various inventive aspects. However, the method of the utility model should not be construed to reflect the intent: rather, the utility model as claimed requires more features than are expressly recited in each claim. Rather, as the following claims reflect, inventive aspects lie in less than all features of a single foregoing inventive embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this invention.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A polymerization reaction apparatus, comprising:
a polymerization reactor (1) connected to a heating device to provide a temperature environment required for polymerization;
the first feeding assembly (2) is arranged on the polymerization reactor (1) to convey materials to be reacted into the polymerization reactor (1), and the materials to be reacted form a pressurized environment higher than atmospheric pressure in the polymerization reactor;
a second feeding assembly (3) comprising: at least one feeding tank (31) which is communicated in sequence, wherein one of the at least one feeding tank (31) is detachably arranged on the polymerization reactor (1) so as to convey catalysts and monomers into the polymerization reactor (1), and the catalysts, the monomers and materials are added into the polymerization reactor in a pressurized environment;
a vacuum assembly (4) in communication with the polymerization reactor (1), the vacuum assembly (4) being arranged to create a vacuum environment within the polymerization reactor (1) prior to input of the material to be reacted into the polymerization reactor (1); and
an isobaric device (5) removably connected between said second feeding assembly (3) and the polymerization reactor (1) to maintain equal pressure inside said feeding tank (31) and the polymerization reactor (1).
2. The polymerization plant according to claim 1, wherein the second feeding assembly (3) further comprises: and the feeding valves (32) are respectively arranged at the input end and the output end of the second feeding assembly (3) and between the two adjacent feeding tanks (31).
3. The polymerization plant according to claim 2, wherein the second feeding assembly (3) further comprises: a first three-way valve (33) disposed at an input of the second feed assembly (3), a first end of the isobaric device (5) being in removable communication with the feed tank (31) through a port of the first three-way valve (33).
4. The polymerization plant according to claim 3, wherein the vacuum assembly (4) comprises a second three-way valve (41), a first port of the second three-way valve (41) communicating with the polymerization reactor (1), a second port communicating with the vacuum assembly (4), and a third port communicating with a second end of the isobaric device (5).
5. The polymerization reaction apparatus according to any one of claims 1 to 4, wherein the first feeding assembly (2) comprises:
a conduit (21) having one end communicating with the polymerization reactor (1);
a gas cylinder communicating with the other end of the conduit (21) and storing an olefin monomer gas; and
and the purification device is communicated with the gas cylinder to provide the olefin monomer gas with qualified impurity content.
6. The polymerization reaction apparatus according to any one of claims 1 to 4,
the polymerization reactor (1) is connected with the first feeding assembly (2) through a quick-connect connector.
7. The polymerization reaction apparatus according to any one of claims 1 to 4, further comprising:
a fixing part (6) provided on the polymerization reactor (1) to mount the polymerization reactor (1) on a support frame.
8. The polymerization reaction apparatus according to any one of claims 1 to 4, further comprising: a pressure gauge (7) disposed on the polymerization reactor (1) to detect a pressure inside the polymerization reactor (1).
9. The polymerization reaction apparatus according to any one of claims 1 to 4, further comprising:
a motor (8) mounted on the polymerization reactor (1); and
the stirring paddle is arranged in the polymerization reactor (1) and is used for stirring the materials in the polymerization reactor (1) under the driving of the motor.
10. The polymerization reaction apparatus according to any one of claims 1 to 4, further comprising:
a pressure sensor (9) arranged on a pipeline communicated with the polymerization reactor (1) and used for detecting and transmitting the pressure inside the polymerization reactor (1);
and the regulating valve (10) is arranged on the pipeline communicated with the polymerization reactor (1) and is used for regulating the internal pressure of the polymerization reactor (1) according to the pressure in the polymerization reactor (1).
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CN202220054266.4U CN216935949U (en) | 2022-01-06 | 2022-01-06 | Polymerization reaction device |
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CN202220054266.4U CN216935949U (en) | 2022-01-06 | 2022-01-06 | Polymerization reaction device |
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