CN210613648U - Microreactor for coordination polymerization of olefin - Google Patents
Microreactor for coordination polymerization of olefin Download PDFInfo
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- CN210613648U CN210613648U CN201920451941.5U CN201920451941U CN210613648U CN 210613648 U CN210613648 U CN 210613648U CN 201920451941 U CN201920451941 U CN 201920451941U CN 210613648 U CN210613648 U CN 210613648U
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Abstract
The utility model relates to a micro-reactor for olefin coordination polymerization, which comprises a feeding module, a main reaction module, a temperature control module and a discharging module; the feeding module is connected with the main reaction module, and the main reaction module is connected with the discharging module; the temperature control module is connected with the main reaction module and is used for controlling the temperature of the main reaction module. The utility model solves the problem of the residence time of the polymerization reaction, so that the catalyst can exert greater efficiency and the polymerization reaction is more thorough; meanwhile, the concentration of olefin monomers in a reaction flow channel tends to be uniform, and the molecular weight and the distribution of the polymer are effectively controlled; in addition, the parallel or serial main reaction modules with independent temperature control can simultaneously prepare a plurality of polymers with different molecular weights and distributions thereof, thereby realizing high-throughput quantification of polymerization. The micro reactor for olefin coordination polymerization is suitable for continuous production and can be used for preparing various polyolefins.
Description
Technical Field
The utility model belongs to the technical field of the reactor, specifically, relate to a micro-reactor for olefin coordination polymerization.
Background
Microreactors have been used in a large number of applications in the production of fine chemicals, biomedicines and nanomaterials and have achieved industrial applications. The flow, transfer and reaction processes are controlled on the scale of tens of microns to thousands of microns, the micro-reactor has extremely high mixing, heat transfer and mass transfer efficiency, and the heat transfer/mass transfer coefficient in the micro-reactor is 1 to 3 orders of magnitude larger than that of the traditional chemical equipment, and is particularly suitable for quick reaction, high exothermic reaction and the like, such as polymerization reaction.
Aiming at the problem that the coordination polymerization of olefin has strict requirements on polymerization reaction conditions, the environment of a micro-reactor system is relatively closed, the high-requirement reaction conditions are easy to realize, the mixing space is small, monomers and a catalyst can be quickly mixed, and the uniformity of the local reaction environment is controlled. Aiming at the problems of violent heat release and easy implosion in the coordination polymerization process of the olefin, the wall surface of a metal reaction pipeline commonly used by a microreactor can make the heat dissipation easier. In addition, aiming at the problems that the pressure of olefin coordination polymerization is generally higher and olefin monomers are inflammable and explosive in industry, the micro-reactor can more easily realize high-grade pressure resistance by adjusting the wall thickness of a pipeline. A plurality of micro reactors are connected in parallel, one reactor has a problem, and can be isolated and treated, so that larger loss can not be caused.
At present, only tubular microreactors (C ANielsen, et al. anal. chem.2002,74,3112; D Beigzadeh, et al. chem.Eng. Technol.2007,30,1088) reported in 2002 by researchers of Dow chemical company are microreactors capable of being applied to olefin coordination polymerization. However, the microreactor has a simple design and has the following problems when it is practically applied to olefin coordination polymerization: 1) in the case of a certain length of the reaction tube, the residence time can only be controlled by the feed pump, which is reduced in accuracy at low flow rates; 2) because the polymer solution has certain viscosity, particularly when a high molecular weight polymer is prepared, the pressure in the system rises along with the increase of the length of a reaction tube, which puts great requirements on equipment; 3) under the feeding condition allowed by the micro-reactor, olefin monomers are continuously consumed along with the extension of a reaction pipeline, the concentration is reduced in a gradient manner, the polymerization growth reaction rate is reduced, and the molecular weight distribution of a polymerization product is widened.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model provides a micro-reactor for olefin coordination polymerization.
The utility model provides a following technical scheme:
a micro-reactor for coordination polymerization of olefin comprises a feeding module, a main reaction module, a temperature control module and a discharging module;
the feeding module is connected with the main reaction module, and the main reaction module is connected with the discharging module; the temperature control module is connected with the main reaction module and is used for controlling the temperature of the main reaction module;
the feeding module comprises a flow divider and a flow dividing flow passage; the arrangement of the flow divider and the flow dividing flow channel can realize multi-point feeding;
the main reaction module comprises a multi-way valve; the multi-way valve can realize multi-stage discharging.
According to an embodiment of the present invention, the number of primary reaction modules is selected from one or more than two;
preferably, when the number of the main reaction modules is more than two, the connection mode between the main reaction modules can be in series or in parallel.
According to an embodiment of the invention, the microreactor optionally comprises or does not comprise a transition means;
according to an embodiment of the present invention, the parallel connection between the main reaction modules is realized by a split flow of the feeding module; the series connection between the main reaction modules is realized by a transition device.
According to an embodiment of the present invention, the number of the feeding module, the main reaction module, the temperature control module, the discharging module may be the same or different, independently selected from one or more than two.
According to an embodiment of the present invention, the plurality of main reaction modules correspond to one or more temperature control modules.
According to the embodiment of the utility model, the two sides of the flow divider are respectively connected with the feed inlet and the discharge outlet; the number of the feed inlets can be 1; the number of the discharge ports can be more than 1, for example more than 2;
preferably, the flow divider is a flow equalizer; preferably, the flow equalizer can be a net structure or a circular hole layout.
According to an embodiment of the present invention, the discharge port of the flow divider is connected to the flow dividing flow passage; preferably, a fastener is arranged between the discharge port and each flow dividing channel; the fastener is connected with the discharge port of the flow divider and each flow dividing flow passage.
According to the embodiment of the present invention, the number of the diversion flow passages may be one, two or more; for example, when the feeding module conveys olefin monomer fluid for feeding, the number of the split flow channels can be more than two; for example, when the feeding module delivers other fluid feeds, the number of the diversion flow channels may be more than one;
preferably, a check valve and/or a stop valve may be disposed in the diversion flow passage.
According to an embodiment of the present invention, the feed module may deliver a gaseous monomer fluid or a liquid monomer fluid feed; preferably, the feeding module of the gas monomer fluid further comprises a filter, a mass flow meter; the feeding module of the liquid monomer fluid also comprises a filter and a high-pressure constant flow pump.
According to an embodiment of the present invention, the main reaction module further comprises a micro mixer, a main reaction flow channel;
preferably, the micromixer may be T-shaped;
preferably, the number of the micromixers may be one, two or more, preferably two or more; preferably, the micromixer is distributed in the main reaction flow channel; preferably, when the number of the micro mixers is more than two, the micro mixers are equidistantly distributed in the main reaction flow channel;
preferably, the number of said multi-way valves may be one, two or more, preferably two or more;
preferably, the multi-way valve is arranged in front of the micro mixer in the main reaction flow channel;
preferably, the multi-way valve may be a three-way valve, and two ends of the three-way valve are connected to the main reaction flow passage, and the other end is connected to another three-way valve through a pipeline.
According to the utility model discloses an embodiment, by the fluid that the reposition of redundant personnel runner flows gets into the main reaction runner after the fluid in micro mixer and the main reaction runner mixes.
According to an embodiment of the present invention, the transition device comprises a receiving container, a constant flow pump and a one-way valve;
preferably, the feed end of the transition device is connected with the discharge port of the multi-way valve of the main reaction module, and the discharge end of the transition device is connected with the micro mixer of the other main reaction module.
According to an embodiment of the present invention, the temperature control module comprises a constant temperature incubator and a cold and hot circulator assembly; the main reaction module is placed in the constant temperature incubator.
According to the utility model, the discharging module comprises a pressure controller and a receiving device; the pressure controller is used for controlling the pressure in the reaction flow channel, and preferably selects a back pressure valve; one end of the pressure controller is connected with the multi-way valve of the main reaction module, and the other end of the pressure controller is connected with the material receiving device.
According to the embodiment of the utility model, the cross sections of the main reaction flow channel and each connecting pipeline are circular, and the pipe wall is uniform; preferably, the tube length of a single main reaction module may be 0.5 to 30m, such as 6m, 8m, 12 m; the outer diameter can be 0.5-10 mm, such as 1.59mm and 3.18 mm; the inner diameter may be 0.2 to 8mm, for example, 0.59mm or 2 mm.
According to the utility model discloses an embodiment, the pipeline material of main reaction flow channel can be at least one in stainless steel, glass, quartzy, PTFE, ETFE, the PEEK.
The utility model has the advantages that:
1. the utility model discloses a micro-reactor for olefin coordination polymerization has realized the series-parallel connection of main reaction module, has solved the problem of polymerization reaction dwell time among the prior art, makes the catalyst performance more efficient, and polymerization is more thorough.
2. The utility model discloses a parallelly connected or the series connection main reaction module of controllable temperature alone can prepare the multiple polymer that has different molecular weight and distribution simultaneously, realizes the high-pass quantification of polymerization. The utility model discloses be fit for continuous production, the amplification effect is little, duplicates the reaction channel of laboratory rank through the subassembly, and parallel can form the reactor of industrial grade each other.
3. The utility model discloses a multi-point feeding can be realized to the feeding module, and its shunt device structure is ingenious, changes tributary quantity and with the hookup location of main reaction runner, can in time effectively regulate and control main reaction runner olefin monomer concentration, has solved the problem that olefin monomer concentration among the prior art reduces along with reaction pipeline length, makes the monomer concentration in the main reaction runner keep at a definite value, is favorable to controlling polymerization product molecular structure and molecular weight.
4. The utility model flexibly adopts the multi-stage discharging module, realizes the control of polymerization reaction time by simply opening and closing the corresponding valve, and is superior to the mode of manually connecting pipelines to adjust the length of the pipe in the prior art; meanwhile, the multi-stage discharging module is favorable for checking the blockage problem in the pipeline.
5. the utility model discloses the accessible is adjusted polymerization dwell time, feeding ratio and multiple feed position etc. and the production molecular structure is clear and definite, controllable multiple polyolefin material of molecular weight, like polyethylene, polypropylene, poly senior alpha-olefin, olefin copolymer etc..
Drawings
FIG. 1 is a schematic structural view of a microreactor according to the present invention;
the system comprises a first feeding module 1, a filter 11, a mass flow meter 12, a flow divider 13, a one-way valve 14, a stop valve 15, a second feeding module 2, a high-pressure constant-flow pump 21, a third feeding module 3, a main reaction module 4, a micro mixer 41, a main reaction flow channel 42, a three-way valve 43, a multi-way valve 44, a transition device 5, a receiving container 51, a high-pressure constant-flow pump 52, a one-way valve 53, a temperature control module 6, a constant-temperature incubator 61, a cold-hot circulator component 62, a discharge module 7, a pressure controller 71 and a material receiving device 72, wherein the mass flow meter is a mass flow meter, the flow divider and the temperature control module 6 are connected with the receiving container 51, the constant-temperature.
Fig. 1 is an exemplary diagram for showing the position relationship of each component, and those skilled in the art can change the number of the components according to the needs, and those skilled in the art can open or close the valve according to the needs of the use to realize the series connection or the parallel connection of the components.
Detailed Description
The present invention will be described in more detail with reference to specific embodiments. It is to be understood that the following examples are only for the purpose of preferably illustrating and explaining the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
As shown in fig. 1, the present embodiment provides a microreactor for coordination polymerization of olefins, which comprises three feeding modules (1, 2, 3), two main reaction modules 4, one temperature control module 6 and two discharging modules 7; the feed module comprises a splitter 13 and ten splitter flow channels.
The first feeding module 1 comprises a splitter 13 and eight splitter flow channels. One end of each split flow channel is connected to the splitter and the other end is connected to the main reaction channel 42 via a micromixer, so that a plurality of feeding points are distributed in the main reaction channel. The olefin-containing monomer fluid is fed by the feed module, so that the monomer concentration in the whole reaction flow channel tends to be uniform.
In this embodiment, the main reaction module 4 includes a micro mixer 41, a main reaction flow passage 42, and a multi-way valve 44.
In this embodiment, the second feeding module 2 includes a high-pressure constant flow pump 21, a flow divider and a flow dividing channel, and the feeding module is responsible for feeding the fluid containing coordination polymerization co-catalyst; the third feeding module 3 comprises a high-pressure constant flow pump, a flow divider and a flow dividing flow channel, and the feeding module is responsible for feeding the fluid containing the coordination polymerization main catalyst;
a first shunting flow channel outlet of the first feeding module 1 and a shunting flow channel outlet of the second feeding module 2 are mixed by a micro mixer and then enter a section of short flow channel; the short runner and the outlet of the flow dividing runner of the third feeding module 3 are mixed by the micro mixer and then enter the main reaction runner 42.
When the gas olefin monomer is fed, a filter 11 and a mass flow meter 12 are arranged in front of the flow divider 13 of the first feeding module 1; the filter is used for removing impurities in the gas; the mass flow meter is used to regulate the feed flow rate of the gaseous olefin monomer.
Each of the split flow paths is provided with a one-way valve 14 and a shut-off valve 15 for stable and selective feeding of liquid fluid.
Except for the first shunt flow channel in the first feeding module 1, the outlets of the other shunt flow channels are mixed with the fluid in the main reaction flow channel through a micro mixer 41 and then enter the main reaction flow channel; the micro mixers are distributed in the main reaction flow channel at equal intervals.
The three-way valve 43 is arranged in front of each micro mixer in the main reaction flow channel, and can selectively discharge before the next olefin monomer feeding point so as to realize multi-stage discharge; the three-way valve has two ends connected to the main reaction flow passage and the other end connected to the multi-way valve 44 via a pipe.
In this embodiment, the microreactor comprises a temperature control module 6.
The temperature control module 6 includes a constant temperature incubator 61 and a thermal cycler assembly 62.
The main reaction module 4 is placed in a constant temperature incubator 61.
The discharging module 7 comprises a pressure controller 71 and a material receiving device 72; one end of the pressure controller 71 is connected with the multi-way valve 44 of the main reaction module, and the other end is connected with the material receiving device 72; the pressure controller is used for controlling the pressure in the reaction flow channel and is a backpressure valve.
The pressure controller 71 is used for adjusting the pressure in the whole reaction flow channel, and further adjusting the polymerization parameters of the olefin monomers; the adjustable range of the pressure controller 71 is 0-3 MPa; the outlet of the pressure controller is connected with the receiving device 72.
In this embodiment, the cross section of the main reaction flow passage 42 is circular, the pipe wall is uniform, the pipe length is 12m, the outer diameter is 1.5mm, and the inner diameter is 0.5 mm.
The main reaction flow passage 42 is made of stainless steel.
Example 2
In contrast to example 1, the microreactor comprises two main reaction modules and is connected in series. Because the polymer solution has a certain viscosity, especially when preparing high molecular weight polymer, the pressure in the system rises along with the increase of the length of the reaction tube, which puts great demands on the equipment. The utility model provides a micro-reactor for alkene coordination polymerization introduces transition device 5 between the main reaction module of establishing ties for solve the problem that the pressure rises along with the increase of reaction tube length in the pipeline.
In the above scheme, the transition device comprises a receiving container 51, a constant flow pump 52 and a one-way valve 53.
One end of the receiving container 51 is connected with the discharge port of the multi-way valve 44 of the first main reaction module 4, and the other end is connected with the feed end of the constant flow pump 52; the feed end of the one-way valve 53 is connected with the discharge end of the constant flow pump 52, and the discharge end of the one-way valve 53 is connected with the feed end of the main reaction flow channel of the second main reaction module.
In the above solution, the first feeding module 1 includes a flow divider 13 and eight flow dividing runners. One end of each flow dividing flow passage is connected with the flow divider, and the other end of each flow dividing flow passage is connected with the main reaction flow passages of the two main reaction modules through the micro mixer, so that a plurality of feeding points are distributed in the main reaction flow passages.
Example 3
In contrast to example 2, the microreactor comprises two temperature control modules.
In the above solution, the temperature control module 6 includes a constant temperature incubator 61 and a cooling and heating cycle machine assembly 62.
The two main reaction modules are respectively placed in the constant temperature insulation boxes of the two temperature control modules.
In this embodiment, by controlling the temperature of each of the serially connected main reaction modules, the molecular-level blending of two polymers having different molecular weights and distributions thereof can be realized, and the polymerization products having different properties can be prepared.
Example 4
In contrast to example 2, the microreactor comprises two feed modules; the first feed module is responsible for the feeding of a liquid olefin monomer-containing and coordination polymerization co-catalyst fluid; the second feed module is responsible for feeding the fluid containing the coordination polymerization procatalyst.
In the above scheme, the first split flow channel outlet of the first feeding module 1 and the first split flow channel outlet of the second feeding module 2 are mixed by a micro mixer and then enter the first main reaction module; and the outlet of the second split flow channel of the first feeding module 1 and the outlet of the second split flow channel of the second feeding module 2 are mixed by a micro mixer and then enter a second main reaction module.
Example 5
Compared with the embodiment 1, the difference is that when the monomer fluid containing liquid olefin is fed, the mass flow meter in front of the splitter 13 of the first feeding module 1 is replaced by a high-pressure constant flow pump; in addition, the present embodiment adopts a parallel mode of two main reaction modules.
In this embodiment, the liquid olefin monomer-containing fluid is a mixed fluid of an olefin monomer and a solvent.
In this embodiment, the parallel connection of the main reaction modules is realized by the flow dividing devices of the feeding modules; the flow dividing device comprises a flow divider and six flow dividing channels.
The first split flow channel outlet of the first feeding module 1 and the first split flow channel outlet of the second feeding module 2 are mixed by a micro mixer and then enter a section of short flow channel; and the short flow channel and the outlet of the first shunting flow channel of the third feeding module 3 are mixed by a micro mixer and then enter the first main reaction module.
The outlet of the second split flow channel of the first feeding module 1 and the outlet of the second split flow channel of the second feeding module 2 are mixed by a micro mixer and then enter a section of short flow channel; and the short flow channel and the outlet of the second split flow channel of the third feeding module 3 are mixed by a micro mixer and then enter the second main reaction module.
Example 6
In contrast to example 5, the microreactor comprises two temperature control modules.
In the above solution, the temperature control module 6 includes a constant temperature incubator 61 and a cooling and heating cycle machine assembly 62.
The two main reaction modules are respectively placed in the constant temperature insulation boxes of the two temperature control modules.
In this embodiment, by controlling the temperature of each of the parallel main reaction modules, two polymers having different molecular weights and distributions thereof can be simultaneously prepared. Based on the design, if a plurality of main reaction modules are connected in parallel, a plurality of polymers with different molecular weights and distributions can be obtained simultaneously. The micro-reactor for olefin coordination polymerization can realize high-throughput polymerization.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement 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 micro-reactor for coordination polymerization of olefins is characterized in that the micro-reactor comprises a feeding module, a main reaction module, a temperature control module and a discharging module;
the feeding module is connected with the main reaction module, and the main reaction module is connected with the discharging module; the temperature control module is connected with the main reaction module and is used for controlling the temperature of the main reaction module;
the feeding module comprises a flow divider and a flow dividing flow passage, and the flow divider and the flow dividing flow passage realize multi-point feeding;
the main reaction module comprises a multi-way valve, and the multi-way valve realizes multi-stage discharging.
2. The microreactor according to claim 1 wherein the number of main reaction modules is selected from one or more than two;
when the number of the main reaction modules is more than two, the main reaction modules are connected in series or in parallel;
the microreactor optionally includes or does not include a transition means;
the parallel connection between the main reaction modules is realized by the shunting of the feeding modules; the series connection between the main reaction modules is realized by a transition device.
3. The microreactor according to claim 1, wherein the number of the feeding modules, the main reaction modules, the temperature control modules and the discharging modules is the same or different and is selected from one or more than two independently from each other;
the plurality of main reaction modules correspond to one or more temperature control modules;
the two sides of the flow divider are respectively connected with a feed inlet and a discharge outlet; the number of the feed inlets is 1; the number of the discharge ports is more than 1;
the discharge port of the flow divider is connected with the flow dividing flow passage; fasteners are arranged between the discharge port and each flow dividing flow passage; the fastener is connected with the discharge port of the flow divider and each flow dividing flow passage.
4. The microreactor according to claim 3, wherein the number of the divided flow channels is one, two or more;
a one-way valve and/or a stop valve is/are arranged in the flow dividing flow passage;
the feed module delivers a gaseous monomer fluid or liquid monomer fluid feed; the feeding module of the gas monomer fluid further comprises a filter and a mass flow meter; the feeding module of the liquid monomer fluid also comprises a filter and a high-pressure constant flow pump.
5. The microreactor of claim 3, wherein the main reaction module further comprises a micromixer, a main reaction flow channel;
the number of the micromixers is one, two or more; the micro mixer is distributed in the main reaction flow passage.
6. The microreactor according to claim 1, wherein the number of multi-way valves is one, two or more;
the multi-way valve is arranged in front of the micro mixer in the main reaction flow channel;
the multi-way valve is a three-way valve, two ends of the three-way valve are connected with the main reaction flow channel, and the other end of the three-way valve is connected with other three-way valves through pipelines.
7. The microreactor according to claim 3 or 5 wherein the fluid flowing out of the divided flow channels is mixed with the fluid in the main reaction flow channel by the micromixer and then enters the main reaction flow channel.
8. The microreactor of claim 2, wherein the transition means comprises a receiving vessel, a constant flow pump and a one-way valve;
the feed end of the transition device is connected with the discharge port of the multi-way valve of the main reaction module, and the discharge end of the transition device is connected with the micro mixer of the other main reaction module.
9. The microreactor of claim 1, wherein the temperature control module comprises a thermostatted incubator and a cold thermal cycler assembly; the main reaction module is placed in the constant-temperature incubator;
the discharging module comprises a pressure controller and a material receiving device; the pressure controller is used for controlling the pressure in the reaction flow channel; one end of the pressure controller is connected with the multi-way valve of the main reaction module, and the other end of the pressure controller is connected with the material receiving device.
10. The microreactor according to claim 5 wherein the cross-section of the main reaction flow channel and each connecting channel is circular and the walls are uniform; the length of the tube of a single main reaction module is 0.5-30 m; the outer diameter is 0.5-10 mm; the inner diameter is 0.2-8 mm.
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| CN201920451941.5U CN210613648U (en) | 2019-04-03 | 2019-04-03 | Microreactor for coordination polymerization of olefin |
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| CN201920451941.5U CN210613648U (en) | 2019-04-03 | 2019-04-03 | Microreactor for coordination polymerization of olefin |
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