CN216856718U - Olefin modular test continuous solution polymerization device - Google Patents
Olefin modular test continuous solution polymerization device Download PDFInfo
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- CN216856718U CN216856718U CN202220358161.8U CN202220358161U CN216856718U CN 216856718 U CN216856718 U CN 216856718U CN 202220358161 U CN202220358161 U CN 202220358161U CN 216856718 U CN216856718 U CN 216856718U
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Abstract
The utility model discloses an olefin modular continuous solution polymerization device, which comprises: a polymerization reaction kettle (1) provided with a pressure gauge (11); a gas feed line (2) connected to the polymerization reactor (1); a liquid feed line (3) connected to the polymerization reactor (1); an exhaust line (4) connected to the polymerization reactor (1) and provided with a first control valve (41) in signal connection with a pressure gauge (11); an overflow tank (5) to which a sensor (51) is attached; an overflow pipeline (6) and a balance pipeline (7) which are connected with the polymerization reaction kettle (1) and the overflow tank (5); and a discharge pipeline (8) connected with the overflow tank (5) and provided with a second control valve (81) in signal connection with the sensor (51). Compared with the prior art, the method has the advantages of simple equipment and easily controlled reaction process.
Description
Technical Field
The utility model relates to the technical field of polyolefin synthesis, in particular to an olefin modular continuous solution polymerization device.
Background
The polyolefin material is composed of ethylene, propylene homopolymer or copolymer obtained by copolymerizing the ethylene, propylene homopolymer, 1-butene, 1-hexene, 1-octene and other alpha-olefins and cycloolefins, and mainly comprises the following components: thermoplastic resins such as High Density Polyethylene (HDPE), Low Density Polyethylene (LDPE), Linear Low Density Polyethylene (LLDPE), polypropylene (PP), and the like; elastomers such as ethylene-propylene rubber (EPR) and ethylene-propylene-diene monomer (EPDM); thermoplastic elastomers such as random copolymers (POE) and block copolymers (OBC) of ethylene and alpha-olefins.
Because of its excellent mechanical properties, chemical stability, processability, easy recovery and low cost, polyolefins are widely used in many fields, and their technical level reflects the state of the art. The polyolefin production process mainly comprises three processes, namely gas phase polymerization, slurry polymerization and solution polymerization. Prior to the advent of metallocene catalysts, the catalysts for the synthesis of polyolefins were mostly heterogeneous catalysts, while the high temperature stability of the conventional Ziegler-Natta catalysts was poor, for which reason most commercial plants of the last century were gas phase and slurry processes. With the rapid development of metallocene catalysts, more and more solution polymerization processes have been applied to polyolefin products. Solution polymerization can produce full density PE, and especially low melting point polymer is more beneficial to comonomer insertion and structure regulation. Even many high value added polyolefin products can be produced almost exclusively by solution polymerization, such as POE and OBC. At present, only two sets of solution polymerization industrial devices are introduced from abroad in 1989 and 1997 for the smooth petrochemical industry and the Jilin petrochemical industry in China, and the domestic solution polymerization process technology is still far behind developed countries. One important reason for slow development is the lack of a sophisticated modeling process for the development of the underlying data.
A mature polyolefin product typically requires a process of mold-pilot-production. The model test device has the characteristics of low cost, flexible operation and small safety risk, and has important significance for mastering the characteristics of the catalyst, the structural design of a product and the development of a process technology. Compared with a large device, the mold testing device has the characteristic of high difficulty in controlling process conditions in the aspect of controlling process parameters, such as unstable retention time, pressure and flow. Most of the reported methods at present tend to full-kettle operation, which is convenient for controlling the residence time of the reaction, but the full-kettle operation has the defects of high equipment requirement, poor safety, incapability of monitoring the composition of components of a polymerization system in time, necessity of keeping the starvation state of the polymerization system for gas-phase monomers and the like.
SUMMERY OF THE UTILITY MODEL
The technical problem to be solved by the present invention is to provide an olefin modular continuous solution polymerization apparatus with simple equipment and easily controlled reaction process, which is particularly suitable for the production of olefin homopolymers and copolymers, such as ethylene/alpha-olefin random copolymer, ethylene/cycloolefin copolymer, etc.
The technical scheme adopted by the utility model for solving the technical problems is as follows: an olefin modular continuous solution polymerization apparatus, comprising:
the polymerization reaction kettle is used for generating polymerization reaction, and a pressure gauge for monitoring the air pressure in an inner cavity of the polymerization reaction kettle is arranged on the polymerization reaction kettle;
a gas feed line for supplying a gas raw material, an outlet end of the gas feed line being connected to the polymerization reaction vessel;
a liquid feed line for supplying a liquid raw material, an outlet end of the liquid feed line being connected to the polymerization reactor;
the inlet end of the exhaust pipeline is connected with the polymerization reaction kettle, and a first control valve for adjusting the flow of the exhaust pipeline is arranged on the exhaust pipeline and is in signal connection with the pressure gauge;
the overflow tank is used for receiving the polymer solution, and a sensor for monitoring the solution amount is arranged on the overflow tank;
the inlet end of the overflow pipeline is connected with the polymerization reaction kettle, and the outlet end of the overflow pipeline is connected with the overflow tank;
the ports at the two ends of the balance pipeline are respectively connected with the polymerization reaction kettle and the overflow tank, and the balance pipeline is positioned above the overflow pipeline and is used for balancing the pressure between the inner cavities of the polymerization reaction kettle and the overflow tank; and
and the inlet end of the discharge pipeline is connected with the overflow tank, a second control valve for adjusting the flow of the discharge pipeline is installed on the discharge pipeline, and the second control valve is in signal connection with the sensor.
In order to control the gas composition in the polymer solution to be constant, the gas feeding pipeline is provided with a flowmeter for detecting the flow of the gas feeding pipeline, the flowmeter is provided with a control valve for controlling the flow of the gas feeding pipeline, and the exhaust pipeline is provided with a detection device for detecting tail gas components in real time.
In order to facilitate the detection device to analyze the components of the tail gas, the gas raw materials comprise reaction gas participating in polymerization reaction and test gas not participating in polymerization reaction. Since the test gas does not participate in the reaction, it is possible to infer the content of the reaction gas by detecting the composition of the test gas.
Preferably, the detection device is a gas chromatograph.
In order to ensure that the tail gas can not enter the detection device under pressure, the detection device is positioned behind the first control valve.
In order to ensure that the gas raw material is fully contacted with the liquid raw material, the outlet end of the gas feeding pipeline extends into the bottom of the inner cavity of the polymerization reaction kettle.
In order to realize the delivery of the liquid raw material, the liquid feeding pipeline is provided with a first delivery pump for delivering the liquid raw material from the inlet to the outlet of the liquid feeding pipeline.
In order to realize the quantitative feeding of the liquid raw materials, the first conveying pump is a metering pump or a peristaltic pump.
In order to inactivate the polymer solution which is uniformly mixed just after the polymer solution is taken out of the kettle, the polymer solution inactivating device further comprises an inactivating agent supply pipeline, and the outlet end of the inactivating agent supply pipeline is connected with the overflow tank.
In order to realize the delivery of the inactivating agent, the inactivating agent supply line is provided with a second delivery pump for delivering the inactivating agent from the inlet to the outlet of the inactivating agent supply line.
Preferably, the sensor is a liquid level sensor or a weight sensor.
Compared with the prior art, the utility model has the advantages that:
(1) the first control valve is arranged on the exhaust pipeline and is in signal connection with a pressure gauge on the polymerization reaction kettle, so that the pressure in the inner cavity of the polymerization reaction kettle can be kept constant;
(2) the overflow tank is additionally arranged, on one hand, the polymerization reaction kettle and the overflow tank are connected through an overflow pipeline, a sensor for monitoring the amount of solution is arranged on the overflow tank and is in signal connection with a second control valve on a discharge pipeline, so that the overflow tank can be always kept in a liquid-carrying state, no gas phase passes through the discharge pipeline, and the continuous discharge of the polymer solution in the overflow tank is maintained;
(3) the reaction gas participating in the polymerization reaction and the test gas not participating in the polymerization reaction form gas raw materials, and the exhaust pipeline is provided with the detection device, so that the detection device can deduce the content of the reaction gas by detecting the composition of the test gas because the test gas does not participate in the reaction, and the gas composition in the polymer solution is controlled to be constant by matching with the flowmeter;
the olefin model continuous solution polymerization device is simple in equipment, can continuously run for several days, is convenient for laboratory product development, provides a ten-kilogram sample required by application testing, can monitor polymerization conditions in a polymerization process, feeds back the polymerization conditions in time, and is suitable for being applied to a model test device.
Drawings
FIG. 1 is a schematic structural view of an embodiment of an olefin modular continuous solution polymerization apparatus according to the present invention;
FIG. 2 is a graph showing the variation of the relevant process parameters of the polymerization reaction in example 1 of the olefin modular continuous solution polymerization process of the present invention.
Detailed Description
The utility model is described in further detail below with reference to the accompanying examples.
As shown in FIG. 1, a preferred embodiment of the olefin modular continuous solution polymerization apparatus of the present invention comprises a polymerization reactor 1, a gas feed line 2, a liquid feed line 3, a vent line 4, an overflow tank 5, an overflow line 6, a balance line 7, a discharge line 8 and a deactivator supply line 9.
Wherein, polymerization 1 is used for taking place polymerization, is equipped with agitating unit in its inner chamber and stirs the reactant, and the pressure gauge 11 that is used for monitoring its inner chamber atmospheric pressure is installed at the top of this polymerization 1.
The gas feeding pipeline 2 is used for supplying gas raw materials, the gas raw materials comprise reaction gas participating in polymerization reaction and test gas not participating in polymerization reaction, the outlet end of the gas feeding pipeline 2 extends into the bottom of the inner cavity of the polymerization reaction kettle 1, a flowmeter 21 used for detecting the flow of the gas feeding pipeline 2 is installed on the gas feeding pipeline 2, and the flowmeter 21 is provided with a control valve used for controlling the flow of the gas feeding pipeline 2, so that quantitative feeding of the gas raw materials is realized. The reaction gas is ethylene, propylene, butylene, hydrogen, etc., the test gas is nitrogen, argon or other inert gas, one or more gas feed lines 2 may be used, and all the gas raw materials may be fed individually or mixed in advance.
The liquid feeding pipeline 3 is used for supplying liquid raw materials, the outlet end of the liquid feeding pipeline 3 is connected to the top of the polymerization reaction kettle 1, a first conveying pump 31 for conveying the liquid raw materials from the inlet to the outlet of the liquid feeding pipeline 3 is installed on the liquid feeding pipeline 3, and the first conveying pump 31 is a metering pump or a peristaltic pump, so that the quantitative feeding of the liquid raw materials is realized. The liquid raw materials comprise solvent, monomer, catalyst and cocatalyst, two or more liquid feeding pipelines 3 can be adopted, and all the liquid raw materials can be fed independently or can be fed after several materials are mixed in advance.
The exhaust pipe line 4 is used for discharging tail gas, and the entry end of this exhaust pipe line 4 is connected at the top of polymerization cauldron 1, installs the first control valve 41 that is used for adjusting exhaust pipe line 4 flow on the exhaust pipe line 4 and is used for the detection device 42 of real-time detection tail gas composition, and this detection device 42 is gas chromatography, because test gas does not participate in the reaction, and it can be through the content of composition inference reaction gas who detects test gas. The first control valve 41 is in signal connection with the pressure gauge 11 so as to keep the pressure in the inner cavity of the polymerization reactor 1 constant; the detection device 42 is located behind the first control valve 41, so that it is ensured that the tail gas does not enter the detection device under pressure, the user can adjust the valve opening of the flow meter 21 according to the test result of the detection device 42, and certainly, the detection device 42 can be in signal connection with the flow meter 21, so that the gas composition in the polymer solution can be adjusted in time.
The overflow tank 5 is used for receiving the polymer solution, and a sensor 51 for monitoring the amount of the solution is mounted on the overflow tank 5, and the sensor 51 is a liquid level sensor or a weight sensor.
The inlet end of the overflow line 6 is connected to the upper part of the polymerization reaction kettle 1, and the outlet end is connected to the top of the overflow tank 5, thereby ensuring the constant volume of the liquid in the polymerization reaction kettle 1.
The two end ports of the balance pipeline 7 are respectively connected with the top of the polymerization reaction kettle 1 and the top of the overflow tank 5, and the balance pipeline 7 is positioned above the overflow pipeline 6 and is used for balancing the pressure between the inner cavities of the polymerization reaction kettle 1 and the overflow tank 5 and maintaining the pressure of the polymerization reaction kettle 1 and the overflow tank 5 to be stable.
The inlet end of the discharge line 8 is connected to the bottom of the overflow tank 5, a second control valve 81 for adjusting the flow rate of the discharge line 8 is installed on the discharge line 8, and the second control valve 81 is in signal connection with the sensor 51. Thus, by weight or liquid level interlocking, the overflow tank 5 can be maintained in a liquid-carrying state all the time, ensuring that no gas phase passes through the discharge line 8, and thus maintaining the continuous discharge of the polymer solution in the overflow tank 5.
The outlet end of the inactivating agent supply line 9 is connected to the top of the overflow tank 5, a second delivery pump 91 for delivering the inactivating agent from the inlet to the outlet of the inactivating agent supply line 9 is installed on the inactivating agent supply line 9, and the second delivery pump 91 is a metering pump or a peristaltic pump, so that the quantitative feeding of the inactivating agent is realized.
The utility model also provides an olefin modular continuous solution polymerization process applying the olefin modular continuous solution polymerization device, which comprises the following steps:
firstly, gas raw materials enter a polymerization reaction kettle 1 through a gas feeding pipeline 2, and liquid raw materials enter the polymerization reaction kettle 1 through a liquid feeding pipeline 3;
secondly, the reaction gas and the liquid raw material are subjected to polymerization reaction in a polymerization reaction kettle 1 to generate polymer solution and tail gas;
thirdly, exhausting tail gas in the polymerization reactor 1 through an exhaust pipeline 4, transmitting a signal to a first control valve 41 to adjust the opening of the valve after a pressure gauge 11 monitors that the pressure in the inner cavity of the polymerization reactor 1 reaches a preset value, keeping the pressure in the inner cavity of the polymerization reactor 1 constant, and keeping the pressure in the inner cavity of an overflow tank 5 constant through a balance pipeline 7; the detection device 42 detects tail gas components in real time and adjusts the gas composition in the polymer solution in time through the opening degree of the control valve of the flowmeter 21;
the polymer solution in the polymerization reaction kettle 1 enters the overflow tank 5 through the overflow line 6, the polymer solution in the overflow tank 5 is conveyed to the downstream through the discharge line 8, and after the sensor 51 monitors that the polymer solution in the overflow tank 5 reaches the preset solution amount, a signal is transmitted to the second control valve 81 to adjust the valve opening of the valve, so that the polymer solution in the overflow tank 5 is continuously discharged.
Example 1:
in this example, the gas feed was fed using one gas feed line 2: the adopted reaction gas is ethylene, the adopted test gas is nitrogen, the ethylene and the nitrogen are mixed with the solvent before entering the reaction kettle for feeding, the feeding rate of the ethylene is 85NL/h, and the feeding rate of the nitrogen is 30 NL/h;
the liquid raw material is fed by three liquid feeding pipelines 3: the organic solvent adopted is Isopar E, the main catalyst adopted is dimethyl silicon bridging group-tetramethyl cyclopentadienyl-tert-butylamino-titanium dichloride, Isopar E is used for preparing solution with the concentration of 40 mu mol/L, and feeding is carried out at the speed of 0.5L/h; the cocatalyst adopts methylaluminoxane, Isopar E is used for preparing a solution with the concentration of 50mmol/L, and feeding is carried out at the speed of 0.4L/h; 1-octene is adopted as a comonomer, Isopar E is used for preparing a solution with the concentration of 1.6mol/L, and feeding is carried out at the speed of 0.4L/h;
continuously carrying out solution polymerization on ethylene and 1-octene in a polymerization reaction kettle with the inner diameter of 108mm, the total volume of the reaction kettle of 2L and the effective polymerization volume of 1L, a stirrer, the polymerization temperature of 120 ℃, the polymerization pressure of 3MPa and the retention time of 30 min.
In this example, the polymerization process reached a steady state after the 5 th residence time, and the apparatus was continuously and normally operated for more than 48 hours, as shown in fig. 2, the temperature, pressure, and flow control were all very stable, indicating that the process was stable and reliable, and could be applied to the research of the olefin model solution polymerization process and the development of products, the melting point of the polymer obtained after steady state was 57.8 ℃, the insertion amount of 1-octene was 12.2 mol%, the weight average molecular weight Mw was 76.2kD,
example 2:
in this example, the gas feed was fed using one gas feed line 2: the adopted reaction gas is ethylene, the adopted test gas is nitrogen, the ethylene and the nitrogen are mixed with the solvent before entering the reaction kettle for feeding, the feeding rate of the ethylene is 30NL/h, and the feeding rate of the nitrogen is 10 NL/h;
the liquid raw material is fed by three liquid feeding pipelines 3: the adopted organic solvent is toluene, the adopted main catalyst is dimethyl silicon bridging group-tetramethyl cyclopentadienyl group-tert-butylamino-titanium dichloride, toluene is used for preparing a solution with the concentration of 40 mu mol/L, and feeding is carried out at the speed of 0.5L/h; the cocatalyst adopts methylaluminoxane, is prepared into a solution with the concentration of 50mmol/L by toluene, and is fed at the speed of 0.4L/h; preparing a solution with the concentration of 4.0mol/L by using norbornene and toluene E as a comonomer, and feeding at the speed of 0.4L/h;
the continuous solution polymerization of ethylene and 1-octene was carried out in a polymerization reactor having an inner diameter of 108mm, a total reactor volume of 2L and an effective polymerization volume of 1L and equipped with a stirrer at a polymerization temperature of 140 ℃ and a polymerization pressure of 0.6 MPa.
In this example, the polymerization process reached a steady state after the 6 th residence time, and the glass transition temperature of the cycloolefin copolymer obtained after the steady state was 138 ℃.
Note: the polymer performance testing procedure was as follows:
(1) the molecular weights (Mw and Mn) and their distribution indices (PDI) of the polymers were determined using high temperature gel permeation chromatography (PL-GPC 220); 1, 2, 4-trichlorobenzene is used as a solvent to prepare 0.1-0.3 wt% of polymer solution at 150 ℃, polystyrene with narrow molecular weight distribution is used as a standard sample to measure at 150 ℃, and the flow rate of the solvent is 1.0 ml/min; the parameter k is 5.91 × 10 for all PS standards-4，α＝0.69；
(2) The melting point (Tm) (glass transition temperature (Tg)) of the copolymer was determined by TA Instruments DSC 25; taking a 5.0-7.0 mg polymer sample, heating to 160 ℃ (260 ℃) at 30 ℃/min, keeping the temperature for 5min to eliminate thermal history, then cooling to-90 ℃ (40 ℃) at 10 ℃/min, keeping the temperature for 3min, heating to 160 ℃ (260 ℃) at a speed of 10 ℃/min, and obtaining the melting point (vitrification temperature) of the polymer from the second heating curve;
(3) average composition of comonomer in copolymer Using carbon Spectroscopy Nuclear magnetism: (13C NMR) was measured at 125 ℃ with an instrument model Bruker AC 400; preparing a polymer into a deuterated o-dichlorobenzene solution with the mass fraction of 10% at 150 ℃, and dissolving in advanceDecomposing for 3 to 4 hours to make the sample solution uniform; the instrument parameters are optimized to be pulse angle of 90 degrees, reverse proton decoupling, pulse delay time of 8s, collection time of 1.3s and spectrum width of 8000Hz, and the average scanning times are not less than 5000 times.
Claims (10)
1. An olefin modular continuous solution polymerization apparatus, comprising:
the polymerization reaction kettle (1) is used for generating polymerization reaction, and a pressure gauge (11) for monitoring the air pressure of an inner cavity of the polymerization reaction kettle (1) is arranged on the polymerization reaction kettle;
a gas feed line (2) for supplying a gas raw material, an outlet end of the gas feed line (2) being connected to the polymerization reaction vessel (1);
a liquid feed line (3) for supplying a liquid raw material, an outlet end of the liquid feed line (3) being connected to the polymerization reaction tank (1);
the exhaust pipeline (4) is used for exhausting tail gas, the inlet end of the exhaust pipeline (4) is connected with the polymerization reaction kettle (1), a first control valve (41) used for adjusting the flow of the exhaust pipeline (4) is installed on the exhaust pipeline (4), and the first control valve (41) is in signal connection with the pressure gauge (11);
an overflow tank (5) for receiving the polymer solution, the overflow tank (5) having a sensor (51) mounted thereon for monitoring the amount of solution;
an inlet end of the overflow pipeline (6) is connected with the polymerization reaction kettle (1), and an outlet end of the overflow pipeline is connected with the overflow tank (5);
the ports at the two ends of the balance pipeline (7) are respectively connected with the polymerization reaction kettle (1) and the overflow tank (5), and the balance pipeline is positioned above the overflow pipeline (6) and used for balancing the pressure between the inner cavities of the polymerization reaction kettle (1) and the overflow tank (5); and
the inlet end of the discharging pipeline (8) is connected with the overflow tank (5), a second control valve (81) used for adjusting the flow of the discharging pipeline (8) is installed on the discharging pipeline (8), and the second control valve (81) is in signal connection with the sensor (51).
2. The apparatus for the modular continuous solution polymerization of olefins according to claim 1, wherein: the gas inlet pipeline (2) is provided with a flow meter (21) for detecting the flow of the gas inlet pipeline (2), the flow meter (21) is provided with a control valve for controlling the flow of the gas inlet pipeline (2), and the exhaust pipeline (4) is provided with a detection device (42) for detecting the components of the exhaust gas in real time.
3. The apparatus for the modular continuous solution polymerization of olefins according to claim 2, wherein: the gas raw materials comprise reaction gas participating in polymerization reaction and test gas not participating in polymerization reaction.
4. The apparatus for the modular continuous solution polymerization of olefins according to claim 2, wherein: the detection device (42) is a gas chromatograph.
5. The apparatus for the modular continuous solution polymerization of olefins according to claim 2, wherein: said detection means (42) being located after said first control valve (41).
6. The apparatus for the modular continuous solution polymerization of olefins according to any of claims 1 to 4, characterized in that: the liquid feeding pipeline (3) is provided with a first conveying pump (31) for conveying the liquid raw materials from the inlet to the outlet of the liquid feeding pipeline (3).
7. The apparatus for the modular continuous solution polymerization of olefins according to claim 6, wherein: the first conveying pump (31) is a metering pump or a peristaltic pump.
8. The apparatus for the modular continuous solution polymerization of olefins according to any of claims 1 to 4, characterized in that: the device also comprises an inactivating agent supply pipeline (9), and the outlet end of the inactivating agent supply pipeline (9) is connected with the overflow tank (5).
9. The apparatus for the modular continuous solution polymerization of olefins according to claim 8, wherein: the inactivating agent supply pipeline (9) is provided with a second conveying pump (91) for conveying the inactivating agent from the inlet to the outlet of the inactivating agent supply pipeline (9).
10. The apparatus for the modular continuous solution polymerization of olefins according to any of claims 1 to 4, characterized in that: the sensor (51) is a liquid level sensor or a weight sensor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114392712A (en) * | 2022-02-22 | 2022-04-26 | 拓烯科技(衢州)有限公司 | Olefin modular continuous solution polymerization device and process |
| CN117619322A (en) * | 2024-01-25 | 2024-03-01 | 拓烯科技(衢州)有限公司 | Cycloolefin copolymer continuous solution polymerization die test device and method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114392712A (en) * | 2022-02-22 | 2022-04-26 | 拓烯科技(衢州)有限公司 | Olefin modular continuous solution polymerization device and process |
| CN117619322A (en) * | 2024-01-25 | 2024-03-01 | 拓烯科技(衢州)有限公司 | Cycloolefin copolymer continuous solution polymerization die test device and method |
| CN117619322B (en) * | 2024-01-25 | 2024-04-30 | 拓烯科技(衢州)有限公司 | Cycloolefin copolymer continuous solution polymerization die test device and method |
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