A microreactor and its use in the synthesis of alkylaluminoxanes

Abstract

The present application provides a kind of micro-reactor and its application in the synthesis of alkylaluminoxane, which changes the flow state of materials by adjusting the parameters such as the number, size, spatial arrangement and shape of the embedded structural member, makes the reaction materials fully contact and uniformly mix, prevents excessive hydrolysis, thereby reducing the generation of solid by-products. Due to the small size of the reactor, the equipment has a small liquid holdup, high heat and mass transfer performance, and the reaction process is more safe and controllable when dealing with such intense exothermic reactions as alkylaluminum hydrolysis, the yield of target product is high and the activity is good. In addition, compared with traditional tank reactors, the reactor is updated more quickly, and the structural parameters can be continuously optimized in experiments, so as to obtain better products.

Description

Technical Field

[0001] This invention relates to the field of alkylaluminoxane preparation technology, and more specifically to a microreactor and its application in the synthesis of alkylaluminoxanes. Background Technology

[0002] The polyolefin industry is an indispensable sector for the healthy operation of the national economy. In recent years, the polyolefin industry has developed rapidly due to the continuous improvement of metallocene catalysts. Alkyl aluminum oxanes are important cocatalysts in many olefin polymerization catalytic systems, including metallocene catalysts and post-transition metal catalysts. In the development of high-performance polyolefin materials, alkyl aluminum oxanes play a crucial role in both tackling key catalyst technologies and innovating polyolefin products. Currently, alkyl aluminum oxanes are the most widely used and most active cocatalysts, and have a broad market demand in olefin polymerization.

[0003] Alkyl aluminum oxanes are low-molecular-weight oligomers obtained through the controlled partial hydrolysis of alkyl aluminum, a rapid and strongly exothermic reaction. The reactant, alkyl aluminum, is an extremely reactive metal compound that burns violently when exposed to air. Ideally, an equimolar reaction between alkyl aluminum and water molecules releases alkanes, yielding a clear alkyl aluminum oxane solution. However, when the local water concentration is too high, the alkyl aluminum and alkyl aluminum oxane further hydrolyze to form a solid precipitate of aluminum hydroxide, resulting in a low yield of alkyl aluminum oxanes. Therefore, extremely high requirements are placed on the control of the reaction and the synthesis equipment. Thus, developing safe and efficient alkyl aluminum oxane production technology is of great significance to the polyolefin industry.

[0004] Currently, industrial methods for synthesizing alkylaluminoxanes can be divided into two main categories: free hydration and crystallization hydration.

[0005] The free hydration method introduces water in different states, such as gas, liquid, and solid, into the reactor. Gaseous water can be introduced by carrying water vapor with an inert gas (US 4937363), solid water by flushing ice (US5087713), and liquid water by atomization or solvent entrainment (CN 102190677 B) to react with a dilute solution of alkyl aluminum in an inert solvent to produce aluminum oxanes. A common characteristic of these methods is the direct reaction between alkyl aluminum and free water. Due to the vigorous reaction, high requirements are placed on process control and equipment. The crystallization hydration method refers to introducing the required water into the reaction system through inorganic salts containing water of crystallization or alkali metal hydroxides (commonly used crystal hydrates include FeSO4·7H2O, Al2(SO4)3·18H2O, LiBr·2H2O, etc.). The reaction between the crystallization water of these inorganic substances and alkyl aluminum is relatively gentle, unlike the vigorous reaction between free water and alkyl aluminum, making reaction control easier. In patent CN 1309724C, a suspension is prepared by reacting crystalline hydrates with an inert organic solvent and continuously fed into a stirred reactor containing an alkylaluminum solution for reaction. The hydrolysis reaction is controlled by regulating the release rate of the water of crystallization. However, this method can lead to problems such as product loss and product contamination. In summary, the reaction between alkylaluminum and water is a violent and highly exothermic reaction. Achieving effective reaction control, obtaining high product yields, reducing the hazards of the production process, and simplifying equipment complexity are the main current trends.

[0006] In recent years, with the continuous development of special processing technologies such as 3D printing, microreactor technology has been widely applied in fields such as biology, pharmaceutical synthesis, and fine chemicals. For the rapid, strongly exothermic reaction of alkylaluminoxane synthesis, microreactor technology can be used to precisely control the reaction through feeding. Therefore, designing a microreactor with a special structure for alkylaluminoxane synthesis is an effective method to improve the yield and selectivity of alkylaluminoxanes. Summary of the Invention

[0007] In view of the problems existing in the prior art, one of the objectives of the present invention is to provide a microreactor that is beneficial to improving the yield of the target product, is safe and controllable, is simple to operate, and has higher heat and mass transfer performance.

[0008] A second objective of this invention is to provide an application of a microreactor, corresponding to one objective, in the synthesis of alkylaluminoxanes.

[0009] A third objective of this invention is to provide a method for synthesizing alkylaluminoxanes corresponding to the above-mentioned objective.

[0010] To achieve one of the above objectives, the technical solution adopted by the present invention is as follows:

[0011] A microreactor, comprising:

[0012] A reaction unit, which has a reaction chamber, is used to provide a reaction site;

[0013] At least one first reactant feed channel connected to the reaction chamber for introducing the first reactant;

[0014] At least one second reactant feed channel communicating with the reaction chamber, for introducing a second reactant capable of reacting with the first reactant; and

[0015] At least one product outlet channel connected to the reaction chamber is provided for discharging the reaction product resulting from the reaction of the first reactant and the second reactant.

[0016] The reaction chamber has a capacity of 1.0 mL to 10.0 mL, preferably 1.5 mL to 4.0 mL; and

[0017] The reaction chamber is provided with an embedded structural component, which is selected from one or more of baffles and stepped protrusions.

[0018] In some preferred embodiments of the present invention, the baffle is selected from at least one of rectangular baffles, square baffles and trapezoidal baffles.

[0019] In some preferred embodiments of the invention, the embedded structural member is connected to the bottom of the reaction chamber.

[0020] According to the present invention, when the embedded structural member is connected to a location other than the bottom, such as the top, uneven mixing of reactants will occur. Therefore, the present invention preferably connects the embedded structural member to the bottom of the reaction chamber.

[0021] In some preferred embodiments of the present invention, the first reactant feed channel and the second reactant feed channel are constructed on the same side wall of the reaction chamber, the product discharge channel is constructed on the side wall opposite to the side wall, and the central axes of the first reactant feed channel, the second reactant feed channel and the product discharge channel are in the same plane.

[0022] In some preferred embodiments of the present invention, the plane containing the central axis of the first reactant feed channel, the second reactant feed channel and the product discharge channel is 0.4 to 0.6 times the height of the reaction chamber, preferably 0.45 to 0.55 times the height of the reaction chamber.

[0023] In some preferred embodiments of the present invention, the angle between the first reactant feed channel and the product discharge channel is greater than 120°, preferably 135° to 155°.

[0024] In some preferred embodiments of the present invention, the angle between the first reactant feed channel and the second reactant feed channel is in the range of 5° to 50°, preferably 25° to 45°.

[0025] In some preferred embodiments of the present invention, the angle between the second reactant feed channel and the product discharge channel is greater than the angle between the first reactant feed channel and the product discharge channel.

[0026] In some embodiments of the present invention, the height of the embedded structural member is 0.1 to 0.8 times the height of the reaction chamber.

[0027] In some preferred embodiments of the present invention, the height of the embedded structural member is 0.4 to 0.6 times the height of the reaction chamber.

[0028] In some embodiments of the present invention, the width of the embedded structural member is 0.1 to 0.8 times the width of the reaction chamber.

[0029] In some preferred embodiments of the present invention, the width of the embedded structural member is 0.15 to 0.3 times the width of the reaction chamber.

[0030] In some preferred embodiments of the present invention, the embedded structural members are configured to be distributed in an array at the bottom of the reaction chamber, with the direction perpendicular to the central axis of the product discharge channel defined as a row and the direction parallel to the central axis of the product discharge channel defined as a column. The number of embedded structural members in each row is no more than 6, preferably 1 to 5, more preferably 2 to 4, and the number of embedded structural members in each column is no more than 4, preferably 1 to 3, more preferably 2 to 3.

[0031] In some preferred embodiments of the present invention, the row spacing in the array formed by the embedded structural members is 1 to 3 mm, and the column spacing is 2 to 7 mm.

[0032] According to the present invention, the row spacing refers to the vertical distance between the central axes of the projections of each row of embedded structural members onto the bottom of the reaction chamber; the row spacing refers to the vertical distance between the central axes of the projections of each column of embedded structural members onto the bottom of the reaction chamber.

[0033] According to the present invention, the projection of the embedded structural member at the bottom of the reaction chamber can be perpendicular to the central axis of the product discharge channel or at a certain angle, preferably at an angle of 5° to 90° toward the reactant inlet, and more preferably at 45° to 60°.

[0034] According to the present invention, in each row of embedded structural members, the angle formed between the projection of each embedded structural member on the bottom of the reaction chamber and the central axis of the product discharge channel is the same.

[0035] In some preferred embodiments of the present invention, the inner diameter of the first reactant feed channel is 1.5 mm to 3.5 mm, preferably 1.6 mm to 3.2 mm.

[0036] According to the present invention, the length of the first reactant feed channel is not particularly limited and can be selected according to actual needs during application.

[0037] In some preferred embodiments of the present invention, the inner diameter of the second reactant feed channel is 1.5 mm to 3.5 mm, preferably 1.6 mm to 3.2 mm.

[0038] According to the present invention, the length of the second reactant feed channel is not particularly limited and can be selected according to actual needs during application.

[0039] In some preferred embodiments of the invention, the reaction chamber is configured to have a regular shape, preferably a cylinder or cuboid.

[0040] According to the present invention, the side parallel to the flow direction of the material is defined as the long side, and the length of the long side is defined as the length.

[0041] According to the present invention, when the reaction chamber is constructed in a gas shape other than a cylinder or cuboid, such as a square, it will be detrimental to the passage of gaseous reactants, thereby causing the gaseous reactants to remain in the reaction chamber.

[0042] In some preferred embodiments of the present invention, when the reaction chamber is constructed as a cylinder, the central axis of the cylinder is perpendicular to the horizontal plane, the base radius is 8mm to 20mm, and the height is 5mm to 15mm; when the reaction chamber is constructed as a cuboid, the length of the cuboid is 20mm to 40mm, the width is 12mm to 20mm, and the height is 5mm to 15mm.

[0043] To achieve the second objective mentioned above, the technical solution adopted by the present invention is as follows:

[0044] The application of a microreactor according to any one of the above embodiments in the synthesis of alkylaluminoxanes.

[0045] To achieve the third objective mentioned above, the technical solution adopted by the present invention is as follows:

[0046] A method for synthesizing alkylaluminoxanes, employing a microreactor as described in any of the above embodiments, includes the following steps:

[0047] S1. Alkyl aluminum is mixed with an inert solvent to obtain the first reactant;

[0048] S2. Disperse liquid water in an inert solvent to obtain a second reactant. Preferably, the dispersion diameter of water in the second reactant is in the range of 100 μm to 800 μm.

[0049] S3. The first reactant is introduced into at least one first reactant feed channel, and the second reactant is introduced into at least one second reactant feed channel, so that the first reactant and the second reactant react in the reaction chamber, thereby obtaining a reaction product containing alkylaluminoxane at the product discharge channel outlet.

[0050] In some preferred embodiments of the present invention, in step S1, the alkylaluminum is selected from one or more of trialkylaluminum, arylalkylaluminum, alkoxyalkylaluminum, and haloalkylaluminum. Preferably, the alkylaluminum is selected from trialkylaluminum, more preferably from trialkylaluminum represented by formula A1R3, wherein R is C1 to C1. 10 The hydrocarbon group is preferably a C1-C6 alkyl group; more preferably one or more of trimethylaluminum, triethylaluminum, and triisobutylaluminum.

[0051] In some preferred embodiments of the present invention, in steps S1 and S2, the inert solvents are the same or different, selected from one or more aromatic hydrocarbons and aliphatic hydrocarbons, preferably C6 to C6. 18 Aromatic hydrocarbons and C4-C 12 One or more of the following aliphatic hydrocarbons, more preferably C6-C6: 12 Aromatic hydrocarbons, more preferably one or more of benzene, toluene, xylene and ethylbenzene, and even more preferably toluene.

[0052] In some preferred embodiments of the present invention, in step S1, the mass concentration of the alkyl aluminum is 1 wt% to 20 wt%, preferably 5 wt% to 12 wt%, based on the total mass of the first reactant; and / or in step S2, the volume ratio of the inert solvent to the liquid water is (50 to 150):1, preferably (75 to 125):1.

[0053] In some preferred embodiments of the present invention, in step S3, the number of the first reactant feed channels is two; and / or the number of the second reactant feed channels is one.

[0054] In some preferred embodiments of the present invention, the flow rate of the first reactant is 0.1 mL / min to 10.0 mL / min, preferably 3.0 mL / min to 8.0 mL / min, and more preferably 2.0 mL / min to 6.0 mL / min.

[0055] In some preferred embodiments of the present invention, in step S3, the molar ratio of water in the second reactant entering the reaction chamber to alkyl aluminum in the first reactant is controlled to be (0.6-1.0):1, preferably (0.65-0.85):1.

[0056] In some preferred embodiments of the present invention, in step S3, the temperature at which the first reactant and the second reactant come into contact is controlled to be -5°C to 35°C, and the contact time is 0.5 min to 5 min.

[0057] According to the present invention, the residence time of the reactants in the reaction chamber can be controlled by controlling the feed flow rate of the reactants, thereby achieving a contact time in the range of 0.5 min to 5 min.

[0058] According to the present invention, in step S2, the process of dispersing liquid water in an inert solvent is carried out by a dispersion device. The structure of the dispersion device and the dispersion method are not particularly limited, as long as the liquid water can be uniformly dispersed in the inert solvent to form uniform monodisperse droplets, and the dispersion diameter of the water after processing by the dispersion device is in the range of 100 to 800 μm.

[0059] The beneficial effects of this invention are at least in the following aspects:

[0060] Firstly, the special design and arrangement of the embedded structural components can change the flow pattern of the reactants after they enter the reactor, greatly promoting the mass transfer and diffusion of the reaction water in the alkyl aluminum solution, ensuring thorough mixing of the various materials, reducing excessive hydrolysis caused by insufficient mixing, and reducing the formation of solids.

[0061] Secondly, the reactor has a smaller volume and lower liquid holdup, making it safer and more controllable than traditional batch reactors. It is also simpler to operate and has higher heat and mass transfer performance.

[0062] Third, the reactor can continuously iterate in experiments by adjusting the structural parameters of the embedded structural components to obtain better structural parameters, thereby obtaining better products. Attached Figure Description

[0063] Figure 1 This is a schematic diagram of the embedded structural component used in Examples 1 and 2.

[0064] Figure 2 This is a front view of the reactor in Example 1.

[0065] Figure 3 This is a top view of the reactor in Example 1.

[0066] Figure 4This is a front view of the reactor in Example 2.

[0067] Figure 5 This is a top view of the reactor in Example 2.

[0068] Figure 6 This is a schematic diagram of the dispersion device used in Example 1.

[0069] Figure descriptions: 1-First reaction material feed channel F1; 2-Second reaction material feed channel F2; 3-First reaction material feed channel F3; 4-First reaction material feed channel F4; 5-Second reaction material feed channel F5; 6-First reaction material feed channel F6; 7-Product discharge channel E1; 8-Product discharge channel E2. Detailed Implementation

[0070] The present invention will be described in detail below through embodiments, but the scope of protection of the present invention is not limited to the following description.

[0071] Unless otherwise specified in the examples, the procedures should be performed under standard conditions or conditions recommended by the manufacturer. Reagents or instruments whose manufacturers are not specified are all commercially available products.

[0072] In the following embodiments, high-speed cameras are used to capture images, and ImageJ is used to extract the Sauter average diameter of the microdroplets to obtain the water droplet dispersion particle size.

[0073] In the following implementation method, the yield is calculated using the following formula:

[0074] Yield = (Amount of methylaluminoxane product / Amount of trimethylaluminum feed) × 100%

[0075] Example 1

[0076] The shape of the embedded structural component used in this embodiment is as follows: Figure 1 The image shows a rectangular baffle. The baffle is 1mm long, 3mm wide, and 4mm high.

[0077] In this embodiment, the reactor's reaction chamber is constructed as a cuboid, with a length of 18 mm, a width of 23 mm, and a height of 0.5 mm, resulting in a total effective volume of 2.2 mL. Two alkylaluminum feed channels (first reactant feed channel F1 and first reactant feed channel F3) are symmetrically distributed. A water feed channel (second reactant feed channel F2) is distributed along the reactor's central axis. The product discharge channel E1 is also distributed along the reactor's central axis and is located on the sidewall opposite to the sidewalls where F1, F2, and F3 are located. The central axes of E1, F1, F2, and F3 are on the same plane. The angle between F1 and F2 is 30°, the angle between F2 and E1 is 0°, and the inner diameter of F1, F2, and F3 is 1.6 mm, with a length of 500 mm. There are a total of 9 embedded structural components. The projection of each embedded structural component at the bottom of the reaction chamber is perpendicular to the central axis of the product discharge channel. They are arranged in 3 rows and 3 columns, with a row spacing of 3.5 mm and a column spacing of 5 mm. All of them are located at the bottom of the reaction chamber.

[0078] After vacuum and nitrogen purging, trimethylaluminum was prepared into a 5 wt% toluene solution and fed into each branch at a flow rate of 4.5 mL / min. Distilled water and toluene were fed into the dispersion unit at flow rates of 100 μL / min and 10 mL / min, respectively. Figure 6 The dispersion apparatus shown disperses distilled water in toluene, resulting in water droplet sizes ranging from 50 to 200 μm. The reaction is carried out in a reactor at room temperature (25°C), maintaining a water-to-aluminum molar ratio of 0.72 throughout the process. The discharged reaction solution is filtered through a sand core funnel and toluene is removed under reduced pressure to obtain a white methylaluminoxane product with a yield of 63.1%.

[0079] Example 2

[0080] The reactor in this embodiment differs from that in Embodiment 1 only in that the projection of the outermost two rows of embedded structural components at the bottom of the reaction chamber forms an angle of 60° with the central axis of the product discharge channel (the angle towards the reactant inlet).

[0081] The reaction ended with a methylaluminoxane yield of 67.2%.

[0082] Example 3

[0083] The only difference from Example 2 is that the concentration of the trimethylaluminum toluene solution was increased to 8 wt%, and distilled water was injected at 160 μL / min when the reaction was started. The concentration of the trimethylaluminum toluene solution and toluene were still delivered at 4.5 mL / min and 12 mL / min respectively, and the water-aluminum molar ratio was maintained at 0.72 throughout the process.

[0084] The reaction ended with a methylaluminoxane yield of 67.6%.

[0085] Examples 4-8

[0086] Examples 4-8 investigated the effect of the shape and number of baffles on the yield. The only difference from Example 1 is the size and arrangement of the baffles, as shown in Table 1 below; the experimental results using the corresponding reactors are also shown in Table 2 below.

[0087] Table 1

[0088]

[0089]

[0090] Example 9

[0091] The reactor in this embodiment differs from that in Embodiment 1 only in that the angle between the first reactive material feed channel F1 and the second reactive material feed channel F2 is 50°.

[0092] Example 10

[0093] The reactor in this embodiment differs from that in Embodiment 1 only in that the angle between the first reactive material feed channel F1 and the second reactive material feed channel F2 is 10°.

[0094] Comparative Example 1

[0095] The reactor used in Comparative Example 1 is basically the same as that in Example 1, except that no embedded structural components are provided in Comparative Example 1.

[0096] Alkyl aluminum compounds were synthesized in the same manner as in Example 1 using the reactor of Comparative Example 1.

[0097] The reaction ended with a methylaluminoxane yield of 45.3%.

[0098] Test Example 1

[0099] The methylaluminoxane synthesized in the above embodiments was used as a co-catalyst for ethylene polymerization experiments.

[0100] The main catalyst used in the polymerization experiment evaluation was a complex composed of pyridine diimine ligand {2,6-di-[(2-methylaniline ethyl)pyridine]} and ferrous chloride, with the following structural formula:

[0101]

[0102] The 250ml polymerization reactor was heated to above 90℃, with the temperature regulated by the jacketed circulating water. After a leak test, vacuuming and nitrogen purging were performed, followed by vacuum baking for 2 hours. The reaction temperature was then adjusted to 50℃, and 50mL of toluene was added as the reaction medium. The concentration of the iron-based main catalyst in the reaction medium was 4×10⁻⁶. -5A certain amount of methylaluminoxane co-catalyst was added at a molar ratio of [Al]:[Fe] = 1000 (mol / L). The ethylene pressure regulating valve was opened, and the reaction pressure was maintained at 0.1 MPa. The polymerization reaction was carried out for 30 min. After gas-liquid-solid separation, the solid phase product was dried and weighed; the liquid phase product was quantitatively analyzed by gas chromatography. The activity was calculated from the total product amount.

[0103] The results are shown in Table 2.

[0104] Comparative Test Example 1

[0105] The procedure was essentially the same as in Test Example 1, except that a methylaluminoxane product (10 wt% toluene solution) manufactured by Albemarle, Inc. was used as a cocatalyst. This product was stored in a sealed environment at -18°C for approximately one year from the production date to the test date.

[0106] The results are shown in Table 2.

[0107] Table 2

[0108]

[0109] Based on the comprehensive experimental results and the comparison of experimental and comparative examples, it can be seen that the alkylaluminoxane synthesis reactor with embedded structural components of the present invention produces alkylaluminoxanes, and the catalytic activity under the same conditions reaches or even exceeds the level of commercial products.

[0110] It should be noted that the embodiments described above are only for explaining the present invention and do not constitute any limitation on the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to the present invention within the scope of the claims, and revisions can be made to the present invention without departing from the scope and spirit of the present invention. Although the present invention described herein relates to specific methods, materials, and embodiments, it does not mean that the present invention is limited to the specific examples disclosed herein; on the contrary, the present invention can be extended to all other methods and applications with the same function.

Claims

1. A microreactor for the synthesis of alkylaluminoxanes, comprising: A reaction unit, which has a reaction chamber, is used to provide a reaction site; At least one first reactant feed channel connected to the reaction chamber for introducing the first reactant; At least one second reactant feed channel connected to the reaction chamber is used to introduce a second reactant capable of reacting with the first reactant; At least one product outlet channel connected to the reaction chamber is provided for discharging the reaction product resulting from the reaction of the first reactant and the second reactant. The capacity of the reaction chamber is 1.0 mL to 10.0 mL; The reaction chamber is provided with an embedded structural component, which is a baffle plate, and the embedded structural component is connected to the bottom of the reaction chamber. The first reactant feed channel and the second reactant feed channel are constructed on the same side wall of the reaction chamber, and the product discharge channel is constructed on the side wall opposite to the side wall, and the central axes of the first reactant feed channel, the second reactant feed channel and the product discharge channel are in the same plane; The angle between the first reactant feed channel and the second reactant feed channel is in the range of 25°~45°; The embedded structural components are configured to be distributed in an array at the bottom of the reaction chamber, with the direction perpendicular to the central axis of the product discharge channel defined as a row and the direction parallel to the central axis of the product discharge channel defined as a column. The number of embedded structural components in each row is 3 to 4, and the number of embedded structural components in each column is 2 to 3.

2. The microreactor according to claim 1, characterized in that, The embedded structural component is a stepped protrusion.

3. The microreactor according to claim 1, characterized in that, The capacity of the reaction chamber is 1.5 mL to 4.0 mL.

4. The microreactor according to claim 1, characterized in that, The baffle is selected from at least one of rectangular baffles, square baffles, and trapezoidal baffles.

5. The microreactor according to claim 1, characterized in that, The plane containing the central axis of the first reactant feed channel, the second reactant feed channel, and the product discharge channel is 0.4 to 0.6 times the height of the reaction chamber from the bottom of the reaction chamber.

6. The microreactor according to claim 5, characterized in that, The plane containing the central axis of the first reactant feed channel, the second reactant feed channel, and the product discharge channel is 0.45 to 0.55 times the height of the reaction chamber from the bottom of the reaction chamber.

7. The microreactor according to claim 1, characterized in that, The angle between the first reactant feed channel and the product discharge channel is greater than 120°; and / or the angle between the first reactant feed channel and the second reactant feed channel is in the range of 5°~50°; and / or the angle between the second reactant feed channel and the product discharge channel is greater than the angle between the first reactant feed channel and the product discharge channel.

8. The microreactor according to claim 7, characterized in that, The angle between the first reactant feed channel and the product discharge channel is 135°~155°.

9. The microreactor according to any one of claims 1 to 8, characterized in that, The height of the embedded structural member is 0.1 to 0.8 times the height of the reaction chamber; and / or the width of the embedded structural member is 0.1 to 0.8 times the width of the reaction chamber.

10. The microreactor according to claim 1, characterized in that, The number of embedded structural components in each row is 3.

11. The microreactor according to claim 1, characterized in that, The number of embedded structural components in each column is 3.

12. The microreactor according to any one of claims 1 to 8, characterized in that, The inner diameter of the first reactant feed channel is 1.5 mm to 3.5 mm; and / or the inner diameter of the second reactant feed channel is 1.5 mm to 3.5 mm; and / or the reaction chamber is constructed to have a regular shape.

13. The microreactor according to claim 12, characterized in that, The inner diameter of the first reactant feed channel is 1.6 mm to 3.2 mm; and / or the inner diameter of the second reactant feed channel is 1.6 mm to 3.2 mm; And / or the reaction chamber is constructed as a cylinder or cuboid.

14. The microreactor according to claim 13, characterized in that, When the reaction chamber is constructed as a cylinder, the central axis of the cylinder is perpendicular to the horizontal plane, the base radius is 8mm~20mm, and the height is 5mm~15mm; when the reaction chamber is constructed as a cuboid, the length of the cuboid is 20mm~40mm, the width is 12mm~20mm, and the height is 5mm~15mm.

15. The application of a microreactor according to any one of claims 1 to 14 in the synthesis of alkylaluminoxanes.

16. A method for synthesizing alkylaluminoxanes, comprising using a microreactor according to any one of claims 1 to 14, and comprising the following steps: S1. Alkyl aluminum is mixed with an inert solvent to obtain the first reactant; S2. Disperse liquid water in an inert solvent to obtain a second reactant, wherein the dispersion diameter of water in the second reactant is in the range of 100 μm to 800 μm; S3. The first reactant is introduced into at least one first reactant feed channel, and the second reactant is introduced into at least one second reactant feed channel, so that the first reactant and the second reactant react in the reaction chamber, thereby obtaining a reaction product containing alkylaluminoxane at the product discharge channel outlet.

17. The synthesis method according to claim 16, characterized in that, In step S1, the alkylaluminum is selected from one or more of trialkylaluminum, arylalkylaluminum, alkoxyalkylaluminum, and haloalkylaluminum; and / or in steps S1 and S2, the inert solvents are the same or different and are selected from one or more of aromatic hydrocarbons and aliphatic hydrocarbons.

18. The synthesis method according to claim 17, characterized in that, In step S1, the alkylaluminum is selected from trialkylaluminum; and / or in steps S1 and S2, the inert solvents are the same or different, and are selected from one or more aromatic hydrocarbons and aliphatic hydrocarbons.

19. The synthesis method according to claim 17, characterized in that, In step S1, the alkylaluminum is selected from trialkylaluminum of formula AlR3, wherein R is C1 to C2. 10 The hydrocarbon group; and / or in steps S1 and S2, the inert solvents are the same or different, selected from C6~C6. 18 Aromatic hydrocarbons and C4~C 12 One or more of aliphatic hydrocarbons.

20. The synthesis method according to claim 17, characterized in that, In step S1, the alkylaluminum is selected from trialkylaluminum of formula AlR3, wherein R is a C1 to C6 alkyl group; and / or in steps S1 and S2, the inert solvents are the same or different, and are selected from C6 to C6. 12 Aromatic hydrocarbons.

21. The synthesis method according to claim 17, characterized in that, In step S1, the alkylaluminum is selected from one or more of trimethylaluminum, triethylaluminum, and triisobutylaluminum; and / or in steps S1 and S2, the inert solvents are the same or different and are selected from one or more of benzene, toluene, xylene, and ethylbenzene.

22. The synthesis method according to claim 21, characterized in that, In steps S1 and S2, the inert solvent is toluene.

23. The synthesis method according to claim 16, characterized in that, In step S1, the total mass of the first reactant is used as the measurement standard, and the mass concentration of the alkyl aluminum is 1wt%~20wt%; and / or in step S2, the volume ratio of the inert solvent to the liquid water is (50~150):

1.

24. The synthesis method according to claim 23, characterized in that, In step S1, the total mass of the first reactant is used as the measurement standard, and the mass concentration of the alkyl aluminum is 5wt%~12wt%; and / or in step S2, the volume ratio of the inert solvent to the liquid water is (75~125):

1.

25. The synthesis method according to claim 16 or 17, characterized in that, In step S3, there are two first reactant feed channels; and / or one second reactant feed channel.

26. The synthesis method according to claim 16 or 17, characterized in that, The flow rate of the first reactant is 0.1 mL / min to 10.0 mL / min.

27. The synthesis method according to claim 26, characterized in that, The flow rate of the first reactant is 3.0 mL / min to 8.0 mL / min.

28. The synthesis method according to claim 16 or 17, characterized in that, In step S3, the molar ratio of water in the second reactant entering the reaction chamber to alkyl aluminum in the first reactant is controlled to be (0.6~1.0):1; and / or the temperature of the contact between the first reactant and the second reactant is controlled to be -5℃~35℃, and the contact time is controlled to be 0.5min~5min.

29. The synthesis method according to claim 28, characterized in that, In step S3, the molar ratio of water in the second reactant entering the reaction chamber to alkyl aluminum in the first reactant is controlled to be (0.65~0.85):1.

Images