Norbornene synthesis reaction device

Abstract

The utility model provides a norbornene synthesis reaction device, which comprises: a reaction bin, which is externally provided with a heating element; the stirring assembly at least comprises a spiral blade rod arranged in the reaction bin, a first stirring blade group is arranged at the bottom end of the stirring assembly, and the spiral blade rod can rotate along the axis of the reaction bin and drives the first stirring blade group to stir, so that a reaction material flowing area is formed in the area at the bottom of the reaction bin; the feeding assembly comprises a plurality of liquid feeding holes and a plurality of gas feeding holes; all the liquid feeding ports are jointly used for feeding a cyclopentadiene solution with the total amount being the first feeding amount into the flowing area, and all the gas feeding ports are jointly used for feeding ethylene gas with the total amount being larger than the second feeding amount into the flowing area; the second feeding amount is the amount of ethylene gas required by the reaction of the cyclopentadiene solution of the first feeding amount to generate the norbornene, and the scheme uses the impinging stream effect of a flowing area and a mode of injecting excessive ethylene, so that the side reaction of the cyclopentadiene is reduced, and the synthesis amount of the norbornene is improved.

Description

Technical Field

[0001] The present application relates to the technical field of norbornene synthesis, and in particular to a norbornene synthesis reaction device. Background Art

[0002] Norbornene is used with α - Olefin copolymerization is the key monomer for the preparation of cycloolefin copolymers (COCs), and is also the main precursor for the preparation of cycloolefin polymer (COP) monomers. Cyclic olefin copolymers and cycloolefin polymers have excellent properties such as low density, low hygroscopicity, high light transmittance, and high refractive index. They are special amorphous thermoplastic polymer materials with extremely high application value in the fields of optics, medical packaging materials, and electronics. Therefore, the production of norbornene monomers is crucial.

[0003] In the prior art, norbornene (NB) is synthesized from a cyclopentadiene solution and ethylene gas under the conditions of a reaction temperature of 200-260°C, a reaction pressure of 4-10 MPa, and an average residence time of 30 minutes. However, since the cyclopentadiene solution is prone to dimerization at room temperature to generate dicyclopentadiene, when entering the reactor for reaction, the mixed dicyclopentadiene will react with the cyclopentadiene to generate tricyclopentadiene. The cyclopentadiene that is originally intended to synthesize norbornene with ethylene is prone to produce side reactions with other substances, thereby reducing the synthesis amount of norbornene. Summary of the invention

[0004] In view of the above-mentioned defects or deficiencies in the prior art, the present application aims to provide a norbornene synthesis reaction device, comprising:

[0005] A reaction kettle, wherein the reaction kettle has a reaction chamber for accommodating reactants, and a heating element is disposed outside the reaction chamber;

[0006] A stirring assembly, the stirring assembly at least comprising a spiral blade rod disposed in the reaction bin, a first stirring blade group being disposed at the bottom end of the spiral blade rod, the spiral blade rod being capable of rotating along the axis of the reaction bin and driving the first stirring blade group to stir, so that the area at the bottom of the reaction bin forms a flow area for the reaction material;

[0007] A feed assembly, the feed assembly comprising a plurality of liquid feed inlets arranged on the reactor and distributed in an array along the circumference of the reactor, and a plurality of gas feed inlets arranged in an array along the circumference of the reactor;

[0008] All of the liquid feed ports are used together to feed a first feed amount of cyclopentadiene solution into the flow region, and all of the gas feed ports are used together to feed a second feed amount of ethylene gas into the flow region, wherein the second feed amount is the amount of ethylene gas required for the first feed amount of cyclopentadiene solution to react to produce norbornene.

[0009] According to the technical solution provided in the embodiment of the present application, the reactor is provided with a plurality of gas feed nozzles, and the gas feed port is formed in the gas feed nozzles.

[0010] According to the technical solution provided in the embodiment of the present application, a liquid feed nozzle is provided below the gas feed nozzle, and the liquid feed port is formed in the liquid feed nozzle.

[0011] According to the technical solution provided in the embodiment of the present application, the number of the gas feed nozzles is 6.

[0012] According to the technical solution provided in the embodiment of the present application, the number of the liquid feed nozzles is 6.

[0013] According to the technical solution provided in the embodiment of the present application, the first stirring blade group includes 6 radial flow paddles, and the extension direction of the radial flow paddles is the radial direction of the reactor.

[0014] According to the technical solution provided in the embodiment of the present application, two axial flow paddles are provided on the spiral blade rod and above the first stirring blade group, and are arranged in sequence along the extension direction of the spiral blade rod.

[0015] According to the technical solution provided in the embodiment of the present application, along the axial direction of the reactor, an auxiliary blade group is provided on both sides of the first stirring blade group, and the flow area of ​​the reaction material is between the auxiliary blade groups on both sides.

[0016] According to the technical solution provided in the embodiment of the present application, the auxiliary blade group includes a plurality of auxiliary propellers whose length is greater than that of the radial flow type propeller.

[0017] According to the technical solution provided in the embodiment of the present application, a liquid overflow port and a gas outlet are further provided on the reactor above the highest line level of the reaction material in the reaction bin.

[0018] In summary, the present application proposes a norbornene synthesis reaction device, comprising: a reactor, wherein the reactor has a reaction chamber for accommodating reactants, and a heating element is arranged outside the reaction chamber; the reactants include a cyclopentadiene solution and ethylene gas; a stirring assembly at least includes a spiral blade rod arranged in the reaction chamber, a first stirring blade group is arranged at the bottom of the spiral blade rod, and the spiral blade rod can rotate along the axis of the reaction chamber and drive the first stirring blade group to stir, so that the area at the bottom of the reaction chamber forms a flow area for the reactants; a feeding assembly includes a plurality of liquid feed ports arranged on the reactor and distributed in an array along the circumference of the reactor, and a plurality of gas feed ports distributed in an array along the circumference of the reactor; all the liquid feed ports are used to feed a total amount of a first feed amount of cyclopentadiene solution into the flow area, and all the gas feed ports are used to feed a total amount of ethylene gas greater than a second feed amount into the flow area, and the second feed amount is the amount of ethylene gas required for the cyclopentadiene solution of the first feed amount to react to generate norbornene.

[0019] Compared with the prior art, the beneficial effect of the present application lies in that: the present application is provided with a plurality of gas feed ports and liquid feed ports distributed in an array in the circumferential direction above and below the flow area of ​​the reaction material formed by stirring of the first stirring blade group, and the ethylene gas ejected from the gas feed port and the cyclopentadiene solution flowing out from the liquid feed port will form an impact flow effect in the flow area of ​​the reaction material. Since the depolymerization of dicyclopentadiene to form cyclopentadiene is a pyrolysis process, when the temperature conditions are reached, the impact flow effect can allow the cyclopentadiene obtained by pyrolysis to react quickly with the excess ethylene ejected from the gas feed port to form norbornene. Since the amount of ethylene exceeds the amount of ethylene gas required for the reaction of the cyclopentadiene solution to form norbornene, the side reactions produced will be reduced, and more norbornene will be synthesized. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of the structure of a norbornene synthesis reaction device provided in an embodiment of the present application;

[0021] Figure 2 This is a schematic diagram of the structure of a top view of a norbornene synthesis reaction device provided in an embodiment of the present application.

[0022] The text annotations in the figure represent:

[0023] 1. Driving motor; 2. First reducer; 3. Second reducer; 4. Reactor; 5. Gas outlet; 6. Liquid overflow port; 7. Axial flow paddle; 8. First stirring blade group; 9. Gas feed port; 10. Liquid feed port; 11. Heating element; 12. Spiral blade rod. DETAILED DESCRIPTION

[0024] The present application is further described in detail below in conjunction with the accompanying drawings and embodiments. It is to be understood that the specific embodiments described herein are only used to explain the relevant invention, rather than to limit the invention. It is also necessary to explain that, for ease of description, only the parts related to the invention are shown in the accompanying drawings.

[0025] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0026] As mentioned in the background technology, in view of the problems in the prior art, this application proposes a norbornene synthesis reaction device, please refer to Figure 1 As shown, including:

[0027] A reaction kettle 4, wherein the reaction kettle 4 has a reaction chamber for containing reaction materials, and a heating element 11 is arranged outside the reaction chamber; specifically, the reaction materials include cyclopentadiene solution and ethylene gas;

[0028] Specifically, the reactor 4 is approximately a cylindrical structure, and the heating element 11 is vertically arranged outside the reaction chamber of the reactor 4. The heating element 11 is used to make the temperature in the reaction chamber reach the temperature of 200-260° C. required for synthesizing norbornene.

[0029] A stirring assembly, the stirring assembly at least comprises a spiral blade rod 12 disposed in the reaction bin, a first stirring blade group 8 being disposed at the bottom end thereof, the spiral blade rod 12 being able to rotate along the axis of the reaction bin and drive the first stirring blade group 8 to stir, so that the area at the bottom of the reaction bin forms a flow area for the reaction material;

[0030] Specifically, a driving assembly is provided at the top of the reactor 4, and the driving assembly includes at least a driving motor 1, a first reducer 2, and a second reducer 3 on the side of the first reducer 2 close to the reactor. The gradient deceleration of the first reducer 2 and the second reducer 3 is used to improve the stability of the driving motor 1 in the process of driving the spiral blade rod 12 to rotate. The spiral blade rod 12 is installed on the output shaft of the driving motor 1.

[0031] Specifically, the formation of the flow area of ​​the reactants is related to the design of the first stirring blade set 8, the rotation speed, the properties of the reactants (such as viscosity, density, etc.), the reaction conditions, etc. In this flow area, the molecules or particles in the solution will be affected by the first stirring blade set 8, resulting in collision, mixing, mass transfer, etc., and such collision and mixing will affect the kinetics of the chemical reaction and the formation of the product.

[0032] A feed assembly, the feed assembly comprising a plurality of liquid feed ports 10 arranged on the reactor 4 and distributed in an array along the circumference of the reactor 4, and a plurality of gas feed ports 9 arranged in an array along the circumference of the reactor 4;

[0033] All of the liquid feed ports 10 are used together to feed a first feed amount of cyclopentadiene solution into the flow region, and all of the gas feed ports 9 are used together to feed a second feed amount of ethylene gas into the flow region, wherein the second feed amount is the amount of ethylene gas required for the first feed amount of cyclopentadiene solution to react to produce norbornene.

[0034] Based on the characteristics of the flow area of ​​the reactants, the present application arranges the gas feed port 9 and the liquid feed port 10 near the flow area so that the cyclopentadiene solution and ethylene gas entering the reaction chamber can collide and mix better in the flow area. In addition, a plurality of gas feed ports 9 and liquid feed ports 10 are arranged in an array distributed circumferentially. This distributed feed can also enable the reactants to collide and mix in all directions, thereby improving the reaction efficiency, uniformity and quality of the products.

[0035] In addition to structural changes to improve reaction efficiency, the feed amount is also optimized. Considering that dicyclopentadiene will react with cyclopentadiene to form tricyclopentadiene, cyclopentadiene that is originally used to synthesize norbornene with ethylene is prone to side reactions with other substances. The side reactions will consume the amount of cyclopentadiene, which will lead to a reduction in the synthesis of norbornene. Therefore, the present application adopts the method of spraying excess ethylene gas, and the excess ethylene and dicyclopentadiene solution form a collision in the flow area. The dicyclopentadiene solution is pyrolyzed from a dicyclic to a monocyclic, and the monocyclopentadiene and ethylene react fully, so that as little monocyclopentadiene as possible contacts with by-products, that is, the occurrence of side reactions is reduced, and the reaction opportunities with cyclopentadiene and ethylene are increased, thereby ensuring the generation of more norbornene.

[0036] In a preferred embodiment, the reactor 4 is provided with a plurality of gas feed nozzles, and the gas feed ports 9 are formed in the gas feed nozzles.

[0037] Specifically, the gas feed nozzle can be integrally formed with the reaction kettle 4 .

[0038] In a preferred embodiment, a liquid feed nozzle is provided below the gas feed nozzle, and the liquid feed port 10 is formed in the liquid feed nozzle.

[0039] Specifically, the liquid feed nozzle can be integrally formed with the reaction kettle 4 .

[0040] Furthermore, the gas feed nozzle and the liquid feed nozzle can be arranged along the radial direction of the reactor 4 (horizontally arranged), or the gas feed nozzle can be arranged obliquely downward, and correspondingly, the liquid feed nozzle can be arranged obliquely upward, both pointing to the flow area of ​​the reactant, and the reactant can be injected into the flow area.

[0041] In a preferred embodiment, the number of the gas feed nozzles is 6.

[0042] In a preferred embodiment, the number of the liquid feed nozzles is 6.

[0043] In a preferred embodiment, the first stirring blade group 8 includes 6 radial flow paddles, and the extension direction of the radial flow paddles is the radial direction of the reactor 4 .

[0044] Specifically, please refer to Figure 2 As shown, based on a large number of experiments and combined with the size of the applicable reactor 4, the feed inlet is set to 6 distributed feeds, and the stirring blades are set to 6, and the synthesis effect is optimal.

[0045] In a preferred embodiment, two axial flow paddles 7 are provided on the spiral blade rod 12 and above the first stirring blade group 8 , and are arranged in sequence along the extending direction of the spiral blade rod 12 .

[0046] Specifically, two axial flow paddles 7 are used to stir the reaction materials in the reaction chamber.

[0047] In a preferred embodiment, along the axis direction of the reactor 4, an auxiliary blade group is provided on both sides of the first stirring blade group 8, and the flow area of ​​the reaction material is between the auxiliary blade groups on both sides.

[0048] In a preferred embodiment, the auxiliary blade set includes a plurality of auxiliary propellers whose length is greater than that of the radial flow type propeller.

[0049] Specifically, since the auxiliary paddles of the auxiliary blade groups on both sides are longer than the radial flow paddles of the first stirring blade group 8, the number of auxiliary paddles can be more than the radial flow paddles, or they can be staggered, so that the auxiliary blade groups on both sides form protection for the flow area, and further protect the reaction of cyclopentadiene and ethylene in the flow area.

[0050] In a preferred embodiment, a liquid overflow port 6 and a gas outlet 5 are further provided on the reactor 4 above the highest line level of the reaction material in the reaction bin.

[0051] Specifically, when the reaction material in the reaction chamber rises above the highest line level, it can overflow from the liquid overflow port 6 to ensure the safety of the reaction, and the gas can be discharged from the gas outlet 5.

[0052] This article uses specific examples to illustrate the principles and implementation methods of this application. The description of the above embodiments is only used to help understand the method and its core ideas of this application. The above is only the preferred implementation method of this application. It should be pointed out that due to the limitations of textual expression and the objective existence of infinite specific structures, ordinary technicians in this technical field can make several improvements, modifications or changes without departing from the principles of the present invention, and can also combine the above technical features in an appropriate manner; these improvements, modifications, changes or combinations, or the direct application of the inventive concept and technical solution to other occasions without improvement, should be regarded as the scope of protection of this application.

Claims

1. A norbornene synthesis reaction device, characterized in that: include: A reaction kettle (4), wherein the reaction kettle (4) has a reaction chamber for accommodating reaction materials, and a heating element (11) is arranged outside the reaction chamber; A stirring assembly, the stirring assembly at least comprising a spiral blade rod (12) arranged in the reaction chamber, a first stirring blade group (8) being arranged at the bottom end thereof, the spiral blade rod (12) being capable of rotating along the axis of the reaction chamber and driving the first stirring blade group (8) to stir, so that the area at the bottom of the reaction chamber forms a flow area for the reaction material; A feed assembly, the feed assembly comprising a plurality of liquid feed ports (10) arranged on the reactor (4) and distributed in an array along the circumference of the reactor (4), and a plurality of gas feed ports (9) distributed in an array along the circumference of the reactor (4); All of the liquid feed ports (10) are used together to feed a first feed amount of cyclopentadiene solution into the flow region, and all of the gas feed ports (9) are used together to feed a second feed amount of ethylene gas into the flow region, wherein the second feed amount is the amount of ethylene gas required for the first feed amount of cyclopentadiene solution to react to produce norbornene.

2. The norbornene synthesis reaction device according to claim 1, characterized in that: The reaction kettle (4) is provided with a plurality of gas feed nozzles, and the gas feed ports (9) are formed in the gas feed nozzles.

3. The norbornene synthesis reaction device according to claim 2, characterized in that: A liquid feed nozzle is provided below the gas feed nozzle, and the liquid feed port (10) is formed in the liquid feed nozzle.

4. The norbornene synthesis reaction device according to claim 3, characterized in that: The number of the gas feed nozzles is 6.

5. The norbornene synthesis reaction device according to claim 4, characterized in that: The number of the liquid feed nozzles is 6.

6. The norbornene synthesis reaction device according to claim 5, characterized in that: The first stirring blade group (8) includes 6 radial flow-type paddles, and the extension direction of the radial flow-type paddles is the radial direction of the reaction kettle (4).

7. The norbornene synthesis reaction device according to claim 1, characterized in that: Two axial flow paddles (7) are arranged in sequence along the extending direction of the spiral blade rod (12) and above the first stirring blade group (8).

8. The norbornene synthesis reaction device according to claim 6, characterized in that: Along the axis direction of the reactor (4), an auxiliary blade group is provided on both sides of the first stirring blade group (8), and the flow area of ​​the reaction material is between the auxiliary blade groups on both sides.

9. The norbornene synthesis reaction device according to claim 8, characterized in that: The auxiliary blade group includes a plurality of auxiliary propellers whose length is greater than that of the radial flow type propeller.

10. The norbornene synthesis reaction device according to claim 1, characterized in that: A liquid overflow port (6) and a gas outlet (5) are also provided on the reaction kettle (4) above the highest line level of the reaction material in the reaction bin.

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