Polyα-olefin production apparatus and production method
The microchannel reactor system addresses low conversion and selectivity issues in poly-α-olefin production by enabling efficient mixing and polymerization, achieving high conversion and selectivity with reduced catalyst use and environmental impact.
Patent Information
- Application Number
- JP2022563900
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-04-20
- Filing Date
- 2021-04-20
- Publication Date
- 2026-02-20
- Estimated Expiration
- 2041-04-20
AI Technical Summary
Conventional methods for producing poly-α-olefins face challenges such as low conversion and selectivity, high catalyst consumption, complex process operations, and environmental concerns, particularly in batch and continuous production processes using BF3 cocatalysts.
An apparatus and method utilizing a microchannel reactor system with a feeding unit, mixer, and post-treatment unit for producing poly-α-olefins, which includes a static mixer and parallel/series configurations for catalyst and raw material delivery, enabling efficient mixing and polymerization with reduced secondary reactions.
The system achieves high conversion and selectivity, flexible mixing, rapid reaction rates, and efficient mass transfer, suitable for large-scale industrial production with reduced catalyst use and environmental impact.
Smart Images

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Abstract
Description
[Technical Field]
[0001] The present invention relates to an apparatus and method for producing polyalphaolefins, and more particularly to an apparatus and method for producing polyalphaolefins using a microchannel reactor. [Background technology]
[0002] Polyα-olefins are typically obtained by the polymerization of one or more linear α-olefins via an oligomerization reaction under the action of a catalyst. Hydrogenated polyα-olefins, obtained by separation and hydrogenation of polyα-olefins, can be used for blending into high-quality synthetic base oils. Polyα-olefin synthetic base oils, also known as PAO synthetic base oils, have a wide range of applications due to their excellent properties, such as high viscosity index, ultra-low pour point, excellent thermal and oxidative stability, and high flash point. PAO synthetic base oils are classified according to their kinematic viscosity at 100°C. Mainstream products include PAO4, PAO6, PAO8, PAO10, PAO40, and PAO100. Among them, low-viscosity PAOs with kinematic viscosities between 4 and 8 cSt at 100°C are the most widely used and are primarily used for blending into various high-grade engine oils. The use of low-viscosity PAOs can extend drain intervals, improve fuel economy, and reduce low-temperature torque loss in engines.
[0003] Conventional methods for producing poly-α-olefins typically use Lewis acid catalysts to allow α-olefins to undergo oligomerization, resulting in the formation of polymers with different degrees of polymerization. Currently, the catalysts used industrially to produce low-viscosity poly-α-olefins are primarily BF3 cocatalysts. Typical production processes involve batch or continuous stirred-tank reactors. In BF3 cocatalyzed oligomerization reactions, the BF3 in the gas phase must be fully dispersed and mixed with the coagent and α-olefin in the liquid phase, where a portion of it dissolves to form the active cationic catalyst, which then initiates the α-olefin oligomerization reaction. The dissolution and interphase mass transfer of BF3 determine the macroscopic reaction rate, conversion, etc. Furthermore, too short a reaction time tends to result in low olefin conversion and low product yield. Too long a reaction time can lead to side reactions of the formed α-olefin oligomers, such as secondary polymerization reactions that increase the degree of polymerization and isomerization reactions that decrease the viscosity index.
[0004] US4045508A discloses a continuous method for preparing poly-α-olefins, which is characterized by combining a stirred reactor and a tubular reactor to control a multi-stage polymerization process. However, this method leads to more secondary polymerization reactions of oligomers, and the content of trimers is greatly reduced.
[0005] CN104370675B discloses a method for producing polyα-olefins in a continuous manner, which involves introducing an α-olefin into a continuous glass microchannel reactor in a continuous manner and carrying out a polymerization reaction in the presence of an aluminum compound catalyst and an auxiliary to produce polyα-olefins. This process consumes a large amount of catalyst and requires a higher reaction temperature.
[0006] In addition, the batch-type stirred tank reaction processes reported in the prior art have drawbacks such as large stirred tank reactor volume, large occupied area, strict requirements for process parameter control, complicated process operation, long reaction time and production period, etc. However, continuous production processes also cannot achieve ideal conversion and selectivity, and the two processes cannot fully treat the catalyst in the product. Therefore, the art needs an apparatus and method for producing α-olefin oligomers with high conversion, high selectivity, simple process, low investment cost, safety and environmental friendliness.
[0007] It should be noted that the information disclosed in the Background section above is intended merely to enhance understanding of the background of the present invention and may therefore include information that does not constitute prior art already known to those skilled in the art. Summary of the Invention
[0008] The present invention provides an apparatus and process for producing polyalphaolefins.
[0009] Specifically, the present invention includes the following aspects.
[0010] In a first aspect, the present invention provides an apparatus for producing polyalphaolefins.
[0011] The apparatus for producing poly-α-olefins according to the present invention comprises an input unit 1, a microchannel reactor 2, and a post-treatment unit 3, which are connected in series, the input unit comprising a mixer and / or a pipeline for delivering an olefin raw material, an auxiliary material, and a BF3 catalyst to the microchannel reactor 2, and the input unit 1 comprises at least a mixer for mixing at least a portion of the auxiliary material and at least a portion of the BF3 catalyst, and a pipeline for separately supplying at least a portion of the BF3 catalyst to the microchannel reactor 2.
[0012] According to the apparatus of the present invention, the mixer in the dosing unit 1 can be a static mixer and / or a dynamic mixer, preferably a static mixer, more preferably a static mixer with enhanced mixing. Optionally, the structure and parameters of the mixer are as follows: the operating temperature is 20-200°C, and the upper limit of the operating pressure does not exceed 20 MPa. When two or more mixers are used, these mixers can be connected in parallel, in series, or both in parallel and in series. The mixer can optionally have a heat exchange layer. The mixer can optionally have a filler, which can be selected from pall rings, ceramic balls, regular fillers, corrugated fillers, wire mesh, or plastic rings.
[0013] In one embodiment of the present invention, according to the apparatus of the present invention, the feeding unit 1 can include a mixer for mixing a part of the BF3 catalyst, a part of the auxiliary material, and a part of the olefin raw material, and a pipeline for passing the remaining BF3 catalyst, the remaining auxiliary material, and the remaining olefin raw material through the microchannel reactor 2 individually based on the type of feedstock (hereinafter also referred to as configuration method 1).
[0014] In one embodiment of the present invention, according to the apparatus of the present invention, optionally, the feeding unit 1 includes a mixer for mixing a part of the BF3 catalyst and all of the auxiliary materials, a pipeline for separately passing the rest of the BF3 catalyst through the microchannel reactor 2, and a pipeline for separately passing all of the olefin raw material through the microchannel reactor 2 (hereinafter also referred to as configuration method 2).
[0015] In one embodiment of the present invention, according to the apparatus of the present invention, the feeding unit 1 optionally includes a mixer for mixing a part of the BF3 catalyst and a part of the auxiliary material, and a pipeline for individually passing the remainder of the BF3 catalyst, the remainder of the auxiliary material, and the entire olefin raw material through the microchannel reactor 2 (hereinafter also referred to as configuration method 3).
[0016] In one embodiment of the present invention, according to the apparatus of the present invention, the feeding unit 1 optionally includes a mixer for mixing a part of the BF3 catalyst, a part of the auxiliary material and the whole of the olefin raw material, and a pipeline for separately passing the rest of the BF3 catalyst and the rest of the auxiliary material through the microchannel reactor 2 (hereinafter also referred to as configuration method 4).
[0017] In one embodiment of the present invention, according to the apparatus of the present invention, the feeding unit 1 optionally includes a mixer for mixing a part of the BF3 catalyst, all of the auxiliary materials and a part of the olefin feedstock, and a pipeline for separately passing the rest of the BF3 catalyst and the rest of the olefin feedstock through the microchannel reactor 2 (hereinafter also referred to as configuration method 5).
[0018] In one embodiment of the present invention, according to the apparatus of the present invention, the feeding unit 1 optionally includes a mixer for mixing a part of the BF3 catalyst, all of the auxiliary materials and all of the olefin raw material, and a pipeline for separately passing the rest of the BF3 catalyst through the microchannel reactor 2 (hereinafter also referred to as configuration method 6).
[0019] In one embodiment of the present invention, according to the apparatus of the present invention, preferably, when the BF3 catalyst, the auxiliary material, and the olefin are mixed in the input unit 1 (i.e., the above-mentioned Configuration Scheme 1, Configuration Scheme 4, Configuration Scheme 5, and Configuration Scheme 6), the input unit 1 comprises a first mixer for mixing any two of the three feedstocks, and a second mixer for mixing the mixture from the first mixer and the remaining one feedstock, wherein the first mixer is in communication with the second mixer, and the second mixer is in communication with the microchannel reactor 2. More preferably, the input unit 1 comprises a first mixer for mixing one of the olefin feedstock and the auxiliary material with the olefin feedstock and a second mixer for further mixing the other of the olefin feedstock and the BF3 gas with the mixture. In one embodiment, the input unit 1 comprises a first mixer for mixing the olefin feedstock with the auxiliary feedstock and a second mixer for mixing the mixture with BF3 gas, or the input unit 1 comprises a first mixer for mixing BF3 gas with the auxiliary feedstock and a second mixer for mixing the mixture with the olefin feedstock. The input unit 1 further comprises a pipeline communicating with the microchannel reactors 2 to which the remainder of the feedstocks are respectively supplied.
[0020] In one embodiment of the present invention, according to the apparatus of the present invention, the input unit 1 preferably comprises a first mixer for mixing a part of the BF3 catalyst and all of the auxiliary feedstock, a second mixer for mixing the stream obtained after mixing in the first mixer and all of the olefin feedstock, and a pipeline for separately passing the rest of the BF3 catalyst to the microchannel reactor 2. In particular, the first mixer communicates with the second mixer, and the second mixer communicates with the microchannel reactor 2.
[0021] According to the apparatus of the present invention, the microchannel reactor 2 can perform microchannel reaction between the mixed stream from the mixer of the input unit and the streams from each of the individual pipelines of the input unit. The number of microchannel reactors 2 can be one or more, preferably one, two, three, four, five, or six. When two or more microchannel reactors 2 are used, these microchannel reactors 2 can be connected in series, in parallel, or in both parallel and series.
[0022] The structure and parameters of the microchannel reactor 2 are as follows: 2 to 10,000 parallel reaction channels, an operating temperature range of -70 to 300°C, a maximum allowable reaction pressure not exceeding 20 MPa, a maximum allowable heat transfer medium pressure not exceeding 10 MPa, a fluid channel volume without mixing insertion of 0.1 to 20,000 L, and a volumetric flow rate of 1 to 50,000 L / h. More preferably, the number of reaction channels is 2 to 5,000, more preferably 2 to 500. For example, the number of reaction channels may be 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, etc. In the microchannel reactor of the present invention, each reaction channel is 1 mm 2 from 150mm 2 and a length of 50 mm to 5000 mm. Preferably, each reaction channel is provided with a mixing element capable of promoting mixing of the reaction stream. The mixing element is an element known in the art that can promote mixing of the reaction stream and enhance turbulence, and may be a mixing disk, as well as the first and second mixing elements of the present invention. Preferably, the microchannel reactor of the present invention comprises a header pipe for introducing reaction gases and branch pipes for distributing the reaction gases to each reaction channel.
[0023] In one embodiment of the present invention, according to the apparatus of the present invention, the preferred microchannel reactor 2 (hereinafter also referred to as the preferred microchannel reactor of the present invention) comprises: a shell 003; a supply region 023, a mixing region 008, a reaction region 009, and a collection region 024 are arranged and communicated successively along a first direction within the shell 003, the shell 003 comprising a supply pipe 002 communicating with the supply region 023 and a discharge pipe 001 communicating with the collection region 024, the mixing region 008 comprising a mixing channel 014 extending along the first direction; a fluid distribution pipe 017, the fluid distribution pipe 017 extending from the exterior of the shell 003 into the mixing channel 014, the fluid distribution pipe 017 being connected to a fluid distributor 016 at the end of the mixing channel 014; The supply pipe 002 is used to input the feedstock from the input unit 1, the fluid distribution pipe 017 is connected to the pipeline for the separate supply of BF3 catalyst of the input unit 1 and can be used to input the BF3 catalyst, and the discharge pipe 001 is connected to the high-pressure separation unit 3.
[0024] In one embodiment of the present invention, there can be two or more feed pipes 002, corresponding to the number of pipelines from the input unit 1, excluding the pipeline for separately feeding the BF3 catalyst. These pipelines include the pipelines for separately feeding the microchannel reactor (excluding the one for separately feeding the BF3 catalyst) and the pipeline for connecting the final stage mixer to the microchannel reactor. In the present invention, the above-mentioned "final stage mixer" refers to the mixer in the input unit 1, in which the feedstock is mixed and then connected to the microchannel reactor through a pipeline.
[0025] In the present invention, the first direction is the flow direction of the stream, which may be a horizontal direction, an upward direction, etc. The upward direction is preferred, and an upward direction from bottom to top is more preferred.
[0026] In one embodiment of the present invention, the mixing region 008 and the supply region 023 can be separated by a first partition plate 019. The first partition plate 019 is provided with a plurality of through-holes, each of which is aligned with a mixing channel 014, and thus the mixing region 008 communicates with the supply region 023.
[0027] In one embodiment of the present invention, according to the apparatus of the present invention, preferably, the feed pipe is connected to the mixer of the dosing unit 1 for dosing a mixture of at least two of at least a part of the olefin feedstock, at least a part of the auxiliary feedstock and at least a part of the BF3 catalyst.
[0028] In one embodiment of the present invention, the fluid distributor is preferably at least one selected from a powder sintered body having micropores, a mesoporous foam material, a wire mesh, and a tube having microslits or micropores.
[0029] Preferably, the fluid distributor is a cylindrical sintered powder body having micropores.
[0030] In one embodiment of the present invention, preferably the fluid distributor has a flow rate of 0.01 cm. 2 -200cm 2 and lengths of 1mm-2000mm.
[0031] In one embodiment of the present invention, the mixing channel has a circular cross section and the mixing channel has a diameter of 0.05 cm 2 -400cm 2 and a length of 50 mm-5000 mm. In the present invention, the length and cross-sectional area of the mixing channel 014 are both greater than the length and cross-sectional area of the fluid distributor 016.
[0032] In one embodiment of the present invention, the mixing region comprises 2 to 100 (preferably 2 to 50, more preferably 2 to 10) mixing channels, and the fluid distribution pipes 017 include a main pipe extending from the outside of the shell to the supply region, and distribution pipes extending from the supply region to each mixing channel 014 with a fluid distributor 016 connected to the end of the distribution pipe.
[0033] In one embodiment of the present invention, in the mixing channel 014, the first mixing element 015 is positioned downstream of the fluid distributor 016.
[0034] In one embodiment of the present invention, the first mixing element 015 includes a main flow section and a diverting flow section that are alternately arranged and communicate with each other along a first direction. The main flow section includes a single main flow channel, and the diverting flow section includes multiple diverting flow channels. Preferably, a collection cavity communicating with the multiple diverting flow channels is located downstream of the diverting flow section. The first mixing element 015 can be formed by joining multiple plate-like elements (the number of which can be 2 to 100, preferably 2 to 50, more preferably 10 to 30) (each having a thickness of approximately 0.2 mm to 10 mm) arranged along the first direction. Each plate-like element may have hollows and cavities corresponding to the main flow channel 0001, the diverting flow channel 0002, and the collection cavity 0003, which is convenient for processing and manufacturing.
[0035] In one embodiment of the present invention, the mixing region may include a first heat exchange cavity 013 disposed within the shell, the mixing channel being disposed within the first heat exchange cavity, and the shell having a first heat exchange medium inlet 004 and a first heat exchange medium outlet 005 in communication with the first heat exchange cavity.
[0036] In one embodiment of the present invention, the volume ratio of the first heat exchange cavity to the mixing channel is 2-50; preferably, the volume ratio of the first heat exchange cavity to the mixing channel is 5-30. In the mixing region 008, the mixing channel 014 and the first heat exchange cavity 013 are isolated from each other and do not communicate with each other, but heat conduction can be achieved between them, and a pipe fitting with good thermal conductivity can be used for the mixing channel 014.
[0037] In one embodiment of the present invention, a transition region 020 is provided between the mixing region and the reaction region, and the transition region comprises a stabilization channel 021 having a constant cross-section and a diffusion channel 022 having a gradually expanding cross-section, arranged and communicating along a first direction, wherein the stabilization channel communicates with the mixing channel and the diffusion channel is connected to the reaction region.
[0038] In one embodiment of the present invention, a discharge pipe 018 that runs outside the shell is connected to the stabilization channel.
[0039] In one embodiment of the present invention, the diffusion channel comprises a diffusion plate having a mesh or slits.
[0040] In one embodiment of the present invention, the transition region 020 is provided with partition plates each having a through hole so that the two ends thereof are isolated from the mixing region 008 (mainly the first heat exchange cavity 013) and the reaction region 009 (mainly the second heat exchange cavity 012), respectively, and are connected to the respective mixing channels 014 and the respective reaction channels 010 through the respective through holes on the respective partition plates, and the diffusion channel 022 and the stabilization channel 021 can be pipe fittings provided between the two partition plates.
[0041] In one embodiment of the present invention, the reaction region includes a plurality of parallel reaction channels extending along a first direction and communicating with a mixing channel via a stabilization channel 021 and a diffusion channel 022. The reaction channels have at least one cross section of a circular, rectangular, or triangular shape. The number of reaction channels is, for example, 2 to 10,000 channels, preferably 2 to 5,000 channels, and more preferably 2 to 500 channels.
[0042] In one embodiment of the present invention, the reaction channel comprises a second mixing element, the second mixing element including a base strip extending along a first direction and a tooth-like element connected to the base strip and extending transversely relative to the base strip; the tooth-like element has at least one of a triangular, an arcuate, a wavy, and a spiral shape. Preferably, the tooth-like element is triangular, one side of the triangle is adjacent to the base strip, one end is connected to the base strip, and the other end is 0.01 mm to 20 mm away from the base strip.
[0043] In one embodiment of the present invention, each of the reaction channels independently comprises a plurality of second mixing elements stacked at intervals (the number of second mixing elements may be 2 to 100, preferably 2 to 50, more preferably 10 to 30), and the tooth-like elements of the second mixing elements are arranged alternately.
[0044] Preferably, the reaction channel has a rectangular cross section and the teeth extend between a pair of opposing sides of the rectangle.
[0045] In one embodiment of the present invention, the reaction channel is 1 mm 2 -150mm 2and a length of 50-5000 mm, the shortest distance between reaction channels is 1-50 mm, the second mixing element has a thickness of 0.1-3 mm, and the spacing between adjacent tooth elements is 1-50 mm; preferably, the reaction channels have a length of 100-3000 mm, the shortest distance between reaction channels is 3-30 mm, the second mixing element has a thickness of 0.2-2 mm, and the spacing between adjacent tooth elements is 1.5-20 mm.
[0046] In one embodiment of the present invention, the reaction zone may comprise a second heat exchange cavity 012 disposed within the shell, the reaction channel being disposed within the second heat exchange cavity, and the shell comprising a second heat exchange medium inlet 006 and a second heat exchange medium outlet 007 in communication with the second heat exchange cavity.
[0047] In one embodiment of the present invention, the volume ratio of the second heat exchange cavity to the reaction channel is 2-50, preferably the volume ratio of the second heat exchange cavity to the reaction channel is 5-30.
[0048] In one embodiment of the present invention, the second heat exchange cavity 012 may be formed mainly by the shell 003, and at two ends, a second partition plate 025 between the reaction region 009 and the collection region 024, and a partition plate between the reaction region 009 and the transition region 020, respectively.
[0049] According to the present invention, post-treatment unit 3 allows for post-treatment of the stream entering therein to produce a polyolefin product, which can be one or more of an adsorption unit, a centrifuge, a sedimentation unit, an alkaline wash unit, a water wash unit, and a gas-liquid separator.
[0050] In one embodiment of the present invention, the apparatus of the present invention removes the catalyst in the stream after adsorption with the adsorbent in the adsorption apparatus to produce a crude polyolefin product, which can be further processed to produce a final polyolefin product. The adsorbent can be one or more of a metal oxide, an ion exchange resin, and an activated bleaching earth. The metal oxide is preferably one or more of potassium oxide, calcium oxide, sodium oxide, magnesium oxide, aluminum oxide, and barium oxide. The adsorption apparatus can be one or more of a fluidized bed, a fixed bed, and a continuous stirred tank.
[0051] In one embodiment of the present invention, the apparatus of the present invention can separate the stream obtained after the polymerization reaction into a light liquid phase and a heavy liquid phase using a settling or centrifugal separator. The light liquid phase is a crude polyolefin product and can be subjected to further post-treatment to produce a final polyolefin product. The heavy liquid phase contains a complex of auxiliary materials, BF3, and unreacted olefin feedstock and can be returned to the input unit or microchannel reactor for reuse. In particular, the centrifugal separator is preferably a centrifuge, which can be one or more of a disc bowl centrifuge, a tubular centrifuge, and a horizontal centrifuge.
[0052] In one embodiment of the present invention, according to the apparatus of the present invention, the alkaline washing unit can pass the stream obtained after the polymerization reaction through an alkaline aqueous solution to remove the catalyst, and the resulting stream is then subjected to water washing, liquid-liquid separation and drying to produce the final polyolefin product.
[0053] In one embodiment of the present invention, according to the apparatus of the present invention, the water wash unit can pass the stream obtained after the polymerization reaction through water to remove the catalyst by water washing, and the resulting stream is then subjected to liquid-liquid separation and drying to produce the final polyolefin product.
[0054] In one embodiment of the present invention, according to the apparatus of the present invention, the gas-liquid separation device can remove the catalyst from the stream obtained after the polymerization reaction by gas-liquid separation, and the liquid phase obtained after gas-liquid separation is then subjected to post-treatment to produce the final polyolefin product. The gas phase (BF3 gas) obtained after gas-liquid separation can be recycled for use.
[0055] According to the apparatus of the present invention, based on the total mass of BF3 in the microchannel reactor 2, the mass ratio of the BF3 catalyst directly supplied to the microchannel reactor 2 to the BF3 catalyst mixed in the mixer of the feeding unit is 90-10:10-90, preferably 80-40:20-60, more preferably 70-50:30-50.
[0056] In the present invention, the total mass of BF3 in the microchannel reactor 2 refers to the total mass of BF3 in complexes formed by complexing with auxiliary materials in the microchannel reactor 2 and free BF3. That is, it refers to the total mass of BF3 in the stream delivered from the final stage mixer of the input unit 1 to the microchannel reactor (total mass of BF3 in complexes and free BF3 in the stream), and the mass of the BF3 catalyst supplied independently to the microchannel reactor. That is, it refers to the total amount of BF3 supplied to the input unit 1 and BF3 supplied individually to the microchannel reactor 2. In the present invention, the BF3 catalyst refers to free BF3 not complexed with auxiliary materials, which is also known as BF3 gas or BF3.
[0057] The apparatus for producing poly-α-olefins of the present invention can be used to synthesize poly-α-olefin synthetic oils. The apparatus of the present invention can realize flexible and rapid mixing of catalysts, auxiliary materials and olefin raw materials, and has the advantages of fast polymerization reaction rate, good mass transfer and heat transfer effect, high reaction conversion rate, good product selectivity, and excellent performance, which is suitable for large-scale industrial production.
[0058] The apparatus for producing poly-α-olefins using the microchannel reactor of the present invention can achieve continuous and efficient mixing of the reaction system, maintain fluids flowing and mixing in a plug flow-like manner, ensure the consistency of the residence time of the reaction fluids as much as possible, and avoid undesirable product selectivity due to the distribution of residence times.
[0059] In a second aspect, the present invention provides a method for producing polyalphaolefins.
[0060] The method for producing poly-α-olefins according to the present invention includes feeding a BF catalyst, auxiliary materials and an olefin raw material into a microchannel reactor through a feeding unit, polymerizing the material in the microchannel reactor, and then post-treating the material to produce a polyolefin product, wherein at least a portion of the auxiliary materials and at least a portion of the BF catalyst are mixed in the feeding unit, and at the same time, at least a portion of the BF catalyst is separately fed into the microchannel reactor.
[0061] According to the process of the present invention, preferably in an input unit, at least a portion of the olefin feedstock, at least a portion of the auxiliary feedstock, and at least a portion of the BF3 catalyst are mixed.
[0062] In one embodiment of the present invention, the olefins in the olefin feedstock are C3 to C 20 One or more α-olefins, preferably C5 to C 15 One or more of the α-olefins, more preferably C7 to C 14 For example, the olefin may be one or more of the α-olefins commonly used in the preparation of PAO synthetic base oils, such as nonene and decene.
[0063] In one embodiment of the present invention, the olefin raw material is a C5 to C6 olefin as a solvent. 20 Alkanes and / or C1-C 20 It may further contain an oxygen-containing compound. 20The mass fraction of alkanes can be 0-80%, preferably 0.5-50%, and most preferably 1-30% relative to the total mass of the olefin feedstock. 20 The mass fraction of oxygen-containing compounds can be 0-20%, preferably 0-10%, and most preferably 0.001-5%. 20 The alkane may be one or more of an n-alkane, an isoalkane, and a cycloalkane; C1-C 20 The oxygen-containing compound may be one or more of an n-alkanol, an isoalcohol, and a ketone. The Fischer-Tropsch olefin feedstock is a C3 to C6 20 α-olefins, C5-C 20 Alkanes and C1-C 20 The mixture of oxygen-containing compounds (i.e., olefin feedstock) can be used.
[0064] In one embodiment of the present invention, the auxiliary material may be a commonly used auxiliary material that can be used as an electron donor for BF3, and may be one or more of alcohols having 1 to 20 carbon atoms, ethers having 1 to 20 carbon atoms, aldehydes having 1 to 20 carbon atoms, ketones having 1 to 20 carbon atoms, esters having 1 to 30 carbon atoms, carboxylic acids having 1 to 20 carbon atoms, and phenols having 1 to 20 carbon atoms, preferably alcohols having 1 to 10 carbon atoms, more preferably alcohols having 3 to 5 carbon atoms, such as one or more of n-propanol, isopropanol, n-butanol, isobutanol, n-pentanol, and isopentanol.
[0065] In one embodiment of the present invention, according to the method of the present invention, the mass ratio of the auxiliary material:olefin feedstock:BF3 catalyst in the total amount in the microchannel reactor is preferably 1:1-1000:1-500 (preferably 1:1-500:1-200, most preferably 1:10-250:1-100). The mass ratio of the auxiliary material:olefin feedstock:BF3 catalyst in the total amount can be the mass ratio of the feedstocks when all the feedstocks are fed to the microchannel reactor, i.e., the ratio of the reaction feedstocks in the stream immediately after the fluid distributor, based on an individual calculation. In the present invention, the mass of the auxiliary material includes the mass of the auxiliary material in the BF3 complex, and the mass of BF3 includes the mass of BF3 in the BF3 complex.
[0066] In one embodiment of the present invention, according to the method of the present invention, in the feeding unit, a part of the BF3 catalyst, a part of the auxiliary material and a part of the olefin feedstock can be mixed and passed through the microchannel reactor, and based on the type of feedstock, the remaining BF3 catalyst, the remaining auxiliary material and the remaining olefin feedstock are passed through the microchannel reactor separately (hereinafter also referred to as feeding method 1).
[0067] In one embodiment of the present invention, according to the method of the present invention, in the feeding unit, a stream obtained by mixing a part of the BF3 catalyst and all of the auxiliary materials can be passed through the microchannel reactor, and the rest of the BF3 catalyst and all of the olefin raw material can be passed through the microchannel reactor separately (hereinafter also referred to as feeding method 2). Preferably, when the part of the BF3 catalyst and all of the auxiliary materials are mixed in a mixer, the speed at which the part of the BF3 catalyst passes through the mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, most preferably 1 to 30,000 L / h, and the speed at which all of the auxiliary materials supplied to the mixer pass through the mixer is 0.01 to 1,000 L / h, preferably 0.1 to 800 L / h, most preferably 0.2 to 500 L / h. The mixture obtained after mixing the part of the BF3 catalyst and all of the auxiliary materials in the mixer is The rate at which the remainder of the BF3 catalyst passes through the microchannel reactor is 0.01 to 2000 L / h, preferably 0.1 to 1600 L / h, and most preferably 0.2 to 1000 L / h, the rate at which the remainder of the BF3 catalyst passes through the microchannel reactor individually is 1 to 150,000 L / h, preferably 5 to 100,000 L / h, and most preferably 10 to 50,000 L / h, and the rate at which the entire olefin raw material passes through the microchannel reactor individually is 10 to 5,000 L / h, preferably 20 to 4,000 L / h, and most preferably 40 to 2,500 L / h.
[0068] In one embodiment of the present invention, according to the method of the present invention, in the feeding unit, the stream obtained by mixing a part of the BF catalyst and a part of the auxiliary material can be passed through the microchannel reactor, and the rest of the BF catalyst, the rest of the auxiliary material and the whole of the olefinic raw material are passed through the microchannel reactor separately (hereinafter also referred to as feeding method 3). Preferably, when a portion of the BF3 catalyst and a portion of the auxiliary materials are mixed in the mixer, the rate at which the portion of the BF3 catalyst passes through the mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, and most preferably 1 to 30,000 L / h, the rate at which the portion of the auxiliary materials pass through the mixer is 0.01 to 800 L / h, preferably 0.1 to 500 L / h, and most preferably 0.2 to 400 L / h, and the rate at which the mixture obtained by mixing a portion of the BF3 catalyst and a portion of the auxiliary materials in the mixer passes through the microchannel reactor is 0.01 to 1,600 L / h, and preferably 0.1 to 500 L / h. The rate at which the remainder of the BF3 catalyst passes individually through the microchannel reactor is preferably 0.1 to 1400 L / h, and most preferably 0.2 to 800 L / h, the rate at which the remainder of the auxiliary materials pass individually through the mixer is 0.01 to 200 L / h, preferably 0.1 to 150 L / h, and most preferably 0.2 to 100 L / h, and the rate at which the entire olefin raw material passes individually through the microchannel reactor is 10 to 5000 L / h, preferably 20 to 4000 L / h, and most preferably 40 to 2500 L / h).
[0069] In one embodiment of the present invention, according to the method of the present invention, the stream obtained by mixing a part of the BF catalyst, a part of the auxiliary material and the whole of the olefin raw material in the feeding unit can be passed through the microchannel reactor, and the remaining BF catalyst and the remaining auxiliary material are passed through the microchannel reactor separately (hereinafter also referred to as feeding method 4). Preferably, when a portion of the BF3 catalyst, a portion of the auxiliary materials, and all of the olefin raw material are mixed in the mixer, the rate at which the portion of the BF3 catalyst passes through the mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, and most preferably 1 to 30,000 L / h, the rate at which the portion of the auxiliary materials pass through the mixer is 0.01 to 800 L / h, preferably 0.1 to 500 L / h, and most preferably 0.2 to 400 L / h, and the rate at which the entire olefin raw material passes through the mixer is 10 to 5,000 L / h, preferably 20 to 4,000 L / h, and most preferably 40 to 2,500 L / h, The rate at which the mixture obtained by mixing a part of the olefin raw material and the whole of the olefin raw material in the mixer passes through the microchannel reactor is 0.01 to 6000 L / h, preferably 0.1 to 4600 L / h, and most preferably 0.2 to 3000 L / h; the rate at which the remainder of the BF3 catalyst passes individually through the microchannel reactor is 1 to 150,000 L / h, preferably 5 to 100,000 L / h, and most preferably 10 to 50,000 L / h; and the rate at which the remainder of the auxiliary raw materials pass individually through the microchannel reactor is 0.01 to 200 L / h, preferably 0.1 to 150 L / h, and most preferably 0.2 to 100 L / h.
[0070] In one embodiment of the present invention, according to the method of the present invention, the stream obtained by mixing part of the BF catalyst, all of the auxiliary materials and part of the olefin raw material in the feeding unit can be passed through the microchannel reactor, and the rest of the BF catalyst and the rest of the olefin raw material are passed through the microchannel reactor separately (hereinafter also referred to as feeding method 5). Preferably, when a portion of the BF3 catalyst, all of the auxiliary materials, and a portion of the olefin raw material are mixed in the mixer, the rate at which the portion of the BF3 catalyst passes through the mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, and most preferably 1 to 30,000 L / h, the rate at which all of the auxiliary materials pass through the mixer is 0.01 to 1,000 L / h, preferably 0.1 to 800 L / h, and most preferably 0.2 to 500 L / h, and the rate at which the portion of the olefin raw material passes through the mixer is 1 to 2,000 L / h, preferably 5 to 1,000 L / h, and most preferably 10 to 500 L / h. The rate at which the mixture obtained by mixing a portion of the olefin raw material in the mixer passes through the microchannel reactor is 0.01 to 3000 L / h, preferably 0.1 to 1800 L / h, and most preferably 0.2 to 1000 L / h; the rate at which the remainder of the BF3 catalyst passes individually through the microchannel reactor is 1 to 150,000 L / h, preferably 5 to 100,000 L / h, and most preferably 10 to 50,000 L / h; and the rate at which the remainder of the olefin raw material passes individually through the microchannel reactor is 9 to 3000 L / h, preferably 15 to 3000 L / h, and most preferably 30 to 2000 L / h).
[0071] In one embodiment of the present invention, according to the method of the present invention, the stream obtained by mixing a part of the BF3 catalyst, all of the auxiliary materials, and all of the olefin raw material in the feeding unit can be passed through the microchannel reactor, and the remainder of the BF3 catalyst can be passed through the microchannel reactor separately (hereinafter also referred to as feeding method 6). Preferably, when the part of the BF3 catalyst, all of the auxiliary materials, and all of the olefin raw material are mixed in the mixer, the rate at which the part of the BF3 catalyst passes through the mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, most preferably 1 to 30,000 L / h, the rate at which all of the auxiliary materials pass through the mixer is 0.01 to 1,000 L / h, preferably 0.1 to 800 L / h, most preferably 0.2 to 500 L / h, and the rate at which all of the olefin raw material pass through the mixer is 10 to 5,000 L / h, preferably 20 The flow rate of the mixture obtained by mixing a part of the BF3 catalyst, all of the auxiliary materials, and all of the olefin raw material in the mixer through the microchannel reactor is 10 to 6000 L / h, preferably 0.1 to 4600 L / h, most preferably 0.2 to 3000 L / h, and the flow rate of the remainder of the BF3 catalyst individually through the microchannel reactor is 1 to 150,000 L / h, preferably 5 to 100,000 L / h, most preferably 10 to 50,000 L / h).
[0072] In one embodiment of the present invention, according to the method of the present invention, preferably, in the charging unit, a part of the BF3 catalyst and all of the auxiliary materials can be subjected to a first mixing in a first mixer, then the stream obtained after the first mixing is subjected to a second mixing with all of the olefinic material in the second mixer, and then the stream obtained after the second mixing is passed through the microchannel reactor, and then the remainder of the BF3 catalyst is passed through the microchannel reactor separately. Preferably, when a portion of the BF3 catalyst and all of the auxiliary materials are subjected to the first mixing in the first mixer, the rate at which the portion of the BF3 catalyst passes through the first mixer is 1 to 100,000 L / h, preferably 1 to 80,000 L / h, most preferably 1 to 30,000 L / h, and the rate at which all of the auxiliary materials pass through the first mixer is 0.01 to 1,000 L / h, preferably 0.1 to 800 L / h, most preferably 0.2 to 500 L / h; then, the stream obtained after the first mixing is subjected to second mixing with all of the olefin raw material in the second mixer, and the rate at which the stream obtained after the first mixing passes through the second mixer is 0.01 to 1,000 L / h, preferably 0.1 to 800 L / h, most preferably 0.2 to 500 L / h. is 0.01 to 2000 L / h, preferably 0.1 to 1600 L / h, most preferably 0.2 to 1000 L / h, the rate at which the whole of the olefin raw material passes through the second mixer is 10 to 5000 L / h, preferably 20 to 4000 L / h, most preferably 40 to 2500 L / h, the rate at which the stream obtained after the second mixing passes through the microchannel reactor is 10 to 7000 L / h, preferably 20 to 5600 L / h, most preferably 40 to 3500 L / h, and the rate at which the remainder of the BF3 catalyst passes individually through the microchannel reactor is 1 to 150,000 L / h, preferably 5 to 100,000 L / h, most preferably 10 to 50,000 L / h.
[0073] In one embodiment of the present invention, according to the method of the present invention, the reaction temperature in the microchannel reactor is preferably 0 to 120°C, preferably 10 to 80°C, more preferably 20 to 60°C. Regarding the method of the present invention, the reaction pressure in the microchannel reactor is preferably 0.01 to 10 MPa, preferably 0.01 to 8 MPa, more preferably 0.1 to 6 MPa. According to the method of the present invention, the residence time of the olefin raw material in the microchannel reactor is preferably 1 to 3600 seconds, preferably 10 to 1800 seconds, more preferably 15 to 1000 seconds.
[0074] According to the method of the present invention, any of the microchannel reactors as described in the first embodiment can be used as the microchannel reactor.
[0075] In one embodiment of the present invention, according to the method of the present invention, the post-treatment method may be one or more of adsorption, centrifugation, precipitation, alkaline washing, water washing, and gas-liquid separation, but is preferably adsorption. The adsorbent in the adsorption method may be one or more of metal oxide, ion exchange resin, activated bleaching earth, and molecular sieve, but is preferably metal oxide, and the metal oxide is preferably one or more of potassium oxide, calcium oxide, sodium oxide, magnesium oxide, aluminum oxide, and barium oxide.
[0076] In one embodiment of the present invention, according to the method of the present invention, preferably when the post-treatment method is precipitation or centrifugation, the precipitation or centrifugation can separate the stream entering the post-treatment unit into a light liquid phase and a heavy liquid phase. The heavy liquid phase contains a complex of the auxiliary feedstock, BF3, and unreacted olefin feedstock, and is optionally returned to the input unit or microchannel reactor to continue feeding in the continuous reaction. The light liquid phase is a crude polyolefin product and can be subjected to further post-treatment.
[0077] According to the process of the present invention, preferably fractionation, hydrogenation, and optional blending operations are carried out on the resulting polyolefin product to obtain a synthetic oil that meets the viscosity grade.
[0078] The method of the present invention has the advantages of fast polymerization reaction rate, good mass transfer and heat transfer effect, high reaction conversion rate, good product selectivity and excellent performance, and is suitable for large-scale industrial production.
[0079] In a third aspect, the present invention provides a method for producing polyalphaolefins using an apparatus as described in the first aspect.
[0080] A method for producing polyα-olefins using any apparatus for producing polyα-olefins described in the first embodiment of the present invention includes: feeding a BF3 catalyst, an auxiliary material and an olefin raw material into a microchannel reactor through an input unit 1, subjecting them to a polymerization reaction in the microchannel reactor, and then post-processing to produce a polyolefin product, wherein at least a part of the auxiliary material and at least a part of the BF3 catalyst are mixed in the input unit 1, and simultaneously, at least a part of the BF3 catalyst is separately fed into a microchannel reactor 2.
[0081] In one embodiment of the present invention, the olefins in the olefin feedstock are C3 to C 20 One or more α-olefins, preferably C5 to C 15 One or more of the α-olefins, more preferably C7 to C 14 For example, the olefin may be one or more of the α-olefins commonly used in the preparation of PAO synthetic base oils, such as nonene and decene.
[0082] In one embodiment of the present invention, the olefin raw material is a C5 to C6 olefin as a solvent. 20 Alkanes and / or C1-C 20 It may further contain an oxygen-containing compound. 20The mass fraction of alkanes can be 0-80%, preferably 0.5-50%, and most preferably 1-30% relative to the total mass of the olefin feedstock. 20 The mass fraction of oxygen-containing compounds can be 0-20%, preferably 0-10%, and most preferably 0.001-5%. 20 The alkane may be one or more of an n-alkane, an isoalkane, and a cycloalkane; C1-C 20 The oxygen-containing compound may be one or more of an n-alkanol, an isoalcohol, and a ketone. The Fischer-Tropsch olefin feedstock is a C3 to C6 20 α-olefins, C5-C 20 Alkanes and C1-C 20 The mixture of oxygen-containing compounds (i.e., olefin feedstock) can be used.
[0083] In one embodiment of the present invention, the auxiliary material may be a commonly used auxiliary material that can be used as an electron donor for BF3, and may be one or more of alcohols having 1 to 20 carbon atoms, ethers having 1 to 20 carbon atoms, aldehydes having 1 to 20 carbon atoms, ketones having 1 to 20 carbon atoms, esters having 1 to 30 carbon atoms, carboxylic acids having 1 to 20 carbon atoms, and phenols having 1 to 20 carbon atoms, preferably alcohols having 1 to 10 carbon atoms, more preferably alcohols having 3 to 5 carbon atoms, such as one or more of n-propanol, isopropanol, n-butanol, isobutanol, n-pentanol, and isopentanol.
[0084] In one embodiment of the present invention, according to the method of the present invention, the mass ratio of the auxiliary material:olefin feedstock:total amount of BF3 catalyst in the microchannel reactor is preferably 1:1-1000:1-500 (preferably 1:1-500:1-200, most preferably 1:10-250:1-100). The mass ratio of the auxiliary material:olefin feedstock:total amount of BF3 catalyst can be the mass ratio of the feedstocks when all the feedstocks are fed to the microchannel reactor, i.e., the ratio of the reaction feedstocks in the stream immediately after the fluid distributor, based on an individual calculation. In the present invention, the mass of the auxiliary material includes the mass of the auxiliary material in the BF3 complex, and the mass of BF3 includes the mass of BF3 in the BF3 complex.
[0085] In one embodiment of the present invention, according to the method of the present invention, the reaction temperature in the microchannel reactor 2 is preferably 0 to 120°C, preferably 10 to 80°C, more preferably 20 to 60°C. Regarding the method of the present invention, the reaction pressure in the microchannel reactor 2 is preferably 0.01 to 10 MPa, preferably 0.01 to 8 MPa, more preferably 0.1 to 6 MPa. According to the method of the present invention, the residence time of the olefin raw material in the microchannel reactor 2 is preferably 1 to 3600 seconds, preferably 10 to 1800 seconds, more preferably 15 to 1000 seconds.
[0086] In one embodiment of the present invention, according to the method of the present invention, based on the total mass of BF3 in the microchannel reactor, the mass ratio of the BF3 catalyst directly supplied to the microchannel reactor 2 to the BF3 catalyst added by mixing in the feeding unit is 90-10:10-90, preferably 80-40:20-60, more preferably 70-50:30-50.
[0087] In one embodiment of the present invention, according to the method of the present invention, the post-treatment method may be one or more of adsorption, centrifugation, precipitation, alkaline washing, water washing, and gas-liquid separation, but is preferably adsorption. The adsorbent in the adsorption method may be one or more of metal oxide, ion exchange resin, activated bleaching earth, and molecular sieve, but is preferably metal oxide, and the metal oxide is preferably one or more of potassium oxide, calcium oxide, sodium oxide, magnesium oxide, aluminum oxide, and barium oxide.
[0088] In one embodiment of the present invention, according to the method of the present invention, preferably when the post-treatment method is precipitation or centrifugation, the precipitation or centrifugation can separate the stream entering the post-treatment unit into a light liquid phase and a heavy liquid phase. The heavy liquid phase contains a complex of the auxiliary feedstock, BF3, and unreacted olefin feedstock, and is optionally returned to the input unit or microchannel reactor to continue feeding in the continuous reaction. The light liquid phase is a crude polyolefin product and can be subjected to further post-treatment.
[0089] According to the process of the present invention, preferably fractionation, hydrogenation, and optional blending operations are carried out on the resulting polyolefin product to obtain a synthetic oil that meets the viscosity grade.
[0090] The method of the present invention can realize flexible and rapid mixing of catalyst, auxiliary raw materials and olefin raw materials, and has the advantages of fast polymerization reaction rate, good mass transfer and heat transfer effect, high reaction conversion rate, good product selectivity and excellent performance, which is suitable for large-scale industrial production.
[0091] The polyα-olefin production method using the preferred microchannel reactor of the present invention can achieve continuous and efficient mixing of the reaction system, maintain fluid flow in a plug flow-like manner, ensure as consistent a residence time of the reaction fluid as possible, and avoid undesirable product selectivity due to a distribution of residence times. [Brief explanation of the drawings]
[0092] [Figure 1] FIG. 1 is a schematic diagram of the apparatus of the present invention. [Figure 2] FIG. 2 is a schematic diagram of the apparatus of the present invention. [Figure 3] FIG. 3 is a schematic diagram of a preferred microchannel reactor of the present invention. [Figure 4] FIG. 4 is a cross-sectional view of a first mixing element according to the present invention. [Figure 5] FIG. 5 is a structural diagram of a second mixing element according to the present invention. [Figure 6] FIG. 6 is a structural diagram of a stack of a plurality of second mixing elements according to the present invention. [Figure 7] FIG. 7 is a schematic diagram of a comparative device of the present invention. DETAILED DESCRIPTION OF THE INVENTION
[0093] [Explanation of symbols] 1: Input unit 2: Microchannel reactor 3: Post-processing unit 01: BF3 gas catalyst inlet 02: Sub-material input port 03: Olefin raw material inlet 001: Exhaust pipe 002: Supply pipe 003: Shell 004: First heat exchange medium inlet 005: First heat exchange medium outlet 006: Second heat exchange medium inlet 007: Second heat exchange medium outlet 008: Mixed area 009: Reaction area 010: Reaction channel 011: Second mixing element 012: Second heat exchange cavity 013: First heat exchange cavity 014: Mixed Channel 015: First mixing element 016:Fluid distributor 017: Fluid distribution pipe 018:Exhaust pipe 019: First partition 020:Transition area 021: Stabilization channel 022: Diffusion Channel 023: Supply area 024: Recovery Area 025: Second partition 0001: Main channel 0002: Branch channel 0003: Recovery cavity 0004: Base Strip 0005: Toothed member [Mode for Carrying Out the Invention] The invention is further explained below by way of example and in conjunction with the accompanying drawings, in which:
[0094] FIG. 1 is a schematic diagram of an apparatus for producing poly-α-olefins according to the present invention. The apparatus comprises an input unit 1, a microchannel reactor 2, and a post-treatment unit 3, which are connected in series. Input unit 1 comprises a mixer 11 for mixing a BF3 catalyst and auxiliary materials, a mixer 12 for mixing the mixture of the BF3 catalyst and auxiliary materials with an olefin material, and a pipeline for separately inputting the BF3 catalyst and the olefin material. One branch of mixer 11 can be connected to mixer 12, and the other branch of mixer 11 can be connected to microchannel reactor 2, which in turn is connected to mixer 12.
[0095] FIG. 2 is a schematic diagram of an apparatus for producing poly-α-olefins according to the present invention. The apparatus comprises an input unit 1, a microchannel reactor 2, and a post-treatment unit 3, which are connected in series. The input unit 1 comprises a mixer 11 for mixing a BF3 catalyst and auxiliary materials, a mixer 12 for mixing the mixture of the BF3 catalyst and auxiliary materials with the olefin raw material, and a pipeline for separately inputting the BF3 catalyst. The mixer 11 is connected to the mixer 12, which is connected to the microchannel reactor 2.
[0096] FIG. 3 is a schematic diagram of a preferred microchannel reactor of the present invention, comprising: a shell 003; a supply region 023, a mixing region 008, a reaction region 009, and a collection region 024 are arranged and communicated successively along a first direction within the shell 003, the shell 003 comprising a supply pipe 002 communicating with the supply region 023 and a discharge pipe 001 communicating with the collection region 024, the mixing region 008 comprising a mixing channel 014 extending along the first direction; Fluid distribution pipe 017: The fluid distribution pipe 017 extends from the exterior of the shell 003 into the mixing channel 014, and the fluid distribution pipe 017 is connected to a fluid distributor 016 at the end of the mixing channel 014.
[0097] The shell 003 is the main vessel for containing the reactants and products, and the feed region 023, mixing region 008, reaction region 009, and collection region 024 are different regions of the interior space of the shell 003 (all of which can store streams), and these regions are linearly arranged so that the reactants (and products) advance linearly. In the present invention, the flow direction of the streams is referred to as the first direction. Preferably, as shown in Figure 3, the shell 003 is arranged so that the first direction is the upward direction, and the feed region 023, mixing region 008, reaction region 009, and collection region 024 are arranged in a bottom-to-top direction.
[0098] The first group of reaction streams (mixed streams from the input unit 1; there may be two or more supply pipes 002, the number of which corresponds to the number of pipelines from the input unit 1, excluding the pipelines for individually supplying the BF3 catalyst) can be supplied into the supply region 023 through the supply pipes 002 on the shell 003. The supply region 023 has a relatively large cavity and can serve as a storage for the first group of reaction streams. The first group of reaction streams in the supply region 023 can enter the adjacent mixing region 008, i.e., the mixing channel 014. The fluid distribution pipe 017 is connected to the pipeline for individually supplying the BF3 catalyst in the input unit 1. Thus, the input of the second group of reaction streams (individually supplied BF3 catalyst) can be provided to the mixing channel 014 through the fluid distribution pipe 017, so that the first group of reaction streams and the second group of reaction streams can be mixed with each other in the mixing channel 014 of the mixing region 008. In particular, a fluid distributor 016 is provided at the outlet end of the fluid distribution pipe 017. The fluid distributor 016 can form the second group of reaction streams into smaller droplets or bubbles, so that the second group of reaction streams can be more uniformly distributed to the first group of reaction streams in the mixing channel 014. In particular, the mixing structure in the mixing channel 014 is more suitable for mixing a liquid phase stream and a gas phase stream. The first group of reaction streams is a liquid phase stream, and the second group of reaction streams is a gas phase stream. The gas phase stream is formed into dispersed microbubbles through the fluid distributor 016, which can increase the contact area with the liquid phase stream and at the same time, can have a greater influence on the liquid phase stream, thereby improving the uniformity of mixing of the two.
[0099] Furthermore, as shown in FIG. 3, the mixing channel 014 is a cavity extending along a first direction, i.e., the mixing channel 014 has a substantially tubular structure, thereby allowing the stream therein to flow along the first direction to form a stable plug flow.
[0100] The preferred microchannel reactor provided by the present invention can achieve continuous and efficient mixing of the reaction streams by designing the structure of the mixing channel and the mixing pattern therein, and at the same time, can maintain the reaction fluids flowing in a plug flow pattern, thereby ensuring the consistency of the residence time of the reaction fluids as much as possible and avoiding undesirable product selectivity due to the distribution of residence time.
[0101] More specifically, the fluid distributor 016 is at least one selected from a microporous sintered powder, a mesoporous foam material, a wire mesh, and a tube with microslits or micropores. The microporous sintered powder can be obtained by sintering powder into a microporous structure using powder metallurgy. The hollow / mesoporous foam material is a hollow microchannel with a network skeleton. The wire mesh is a microporous network structure. The tube has microslits or microholes. All of these can disperse the fluid from the fluid distribution pipe 017 into smaller bubbles or droplets.
[0102] Preferably, the fluid distributor 016 is a cylindrical sintered powder body having micropores, and the mixing channel 014 has a circular cross section. The fluid distributor 016 may have a structure having substantially the same outer diameter as the fluid distribution pipe 017, and the cross-sectional shape of the fluid distributor 016 substantially corresponds to the cross-sectional shape of the mixing channel 014. The fluid distributor 016 is arranged coaxially with the mixing channel 014 so as to enable the fluid stream dispersed by the fluid distributor 016 to be more uniformly mixed with the stream in the mixing channel 014, forming a stable and uniform plug flow and avoiding mismatch in the residence time of the stream.
[0103] In particular, the fluid distributor 016 has a diameter of 0.01 cm 2 -200cm 2The mixing channel 014 has a cross-sectional area of 0.05 cm 2 -400cm 2 and a length of 50 mm-5000 mm. The length and cross-sectional area of the mixing channel 014 are both greater than the length and cross-sectional area of the fluid distributor 016.
[0104] The mixing zone 008 further includes 2 to 100 (preferably 2 to 50, more preferably 2 to 10) mixing channels 014. The fluid distribution pipe 017 includes a main pipe extending from the outside of the shell 003 into the feed zone 023 and a branch pipe extending from the feed zone 023 into each mixing channel 014, with the branch pipe having a fluid distributor 016 connected to the end of the branch pipe. Each of the multiple mixing channels 014 is connected to the feed zone 023, and the first group of reaction streams is divided into multiple parts within the mixing channel, which serves to disperse the first group of reaction streams, allowing the first group of reaction streams to form a stable, uniform plug flow. The fluid distribution pipe 017 includes a main pipe and a branch pipe. The main pipe is connected to a pipeline for individually supplying the BF catalyst to the dosing unit 1 and extends from a position in the shell 003 corresponding to the feed zone 023 into the feed zone 023. The branch pipe extends from the feed zone 023 into the mixing channel 014. That is, the fluid distribution pipe 017 extends from the feed region 023 into the mixing channel 014. The mixing region 008 and the feed region 023 can be separated by a first partition plate 019. The first partition plate 019 is provided with a plurality of through-holes, and each mixing channel 014 is aligned with each through-hole, so that the mixing region 008 communicates with the feed region 023.
[0105] Furthermore, in the mixing channel 014, the first mixing element 015 is disposed downstream of the fluid distributor 016. In the mixing channel 014, downstream of the fluid distributor 016 refers to the downstream position in the fluid flow direction (i.e., downstream of the fluid distributor 016 in the first direction), i.e., a position closer to the reaction zone 009 than the fluid distributor 016. Through the first mixing element 015, the fluids can be further mixed to improve the mixing uniformity of the two groups of streams.
[0106] Specifically, the first mixing element 015 has main flow sections and branch flow sections that are alternately arranged and communicate with each other along a first direction. The main flow section has one main flow section 0001, and the branch flow section has multiple branch flow sections 0002. As shown in FIG. 4, one or more main flow sections / branch flow sections may be provided and alternately arranged, with only one main flow section 0001 arranged in the main flow section and multiple branch flow sections 0002 arranged in the branch flow section. The fluid converges into the main flow section 0001 and disperses into the branch flow sections 0002 of each branch flow section. This confluence and dispersion process can sufficiently increase the degree of turbulence and improve the uniformity of fluid mixing.
[0107] Furthermore, in the first mixing element 015, a collection cavity 0003 communicating with the plurality of branch channels 0002 is disposed downstream of the branch flow section 0002. As shown in Fig. 4, the volume (particularly the cross-sectional area) of the collection cavity 0003 is larger than the volume (particularly the cross-sectional area) of the main channel 0001, and the collection cavity 0003 can merge the plurality of upstream branch channels 0002, and communicates with the next main channel 0001, or the next stage of the reaction region 009 or the transition region 020.
[0108] As shown in FIG. 4, a first mixing element 015 according to an embodiment of the present invention is shown, and the first mixing element 015 is formed by splicing together a plurality of plate elements (2 to 100, preferably 2 to 50, more preferably 10 to 30) (with a thickness of approximately 0.2 mm to 10 mm) arranged along a first direction, and each plate element has a hollow structure and a cavity corresponding to a main flow path 0001, a branch flow path 0002, and a collection cavity 0003, which is convenient for processing and manufacturing.
[0109] Furthermore, the mixing region 008 includes a first heat exchange cavity disposed within the shell 003, the mixing channel 014 is disposed within the first heat exchange cavity 013, and the shell 003 has a first heat exchange medium inlet 004 and a first heat exchange medium outlet 005 communicating with the first heat exchange cavity 013. In the mixing region 008, the mixing channel 014 and the first heat exchange cavity 013 are isolated from each other and do not communicate with each other, but can achieve heat conduction with each other, and a pipe fitting with good thermal conductivity can be used for the mixing channel 014. By supplying the heat exchange medium to the first heat exchange medium inlet 004 and discharging the heat exchange medium through the first heat exchange medium outlet 005, a circulating flow of the heat exchange medium can be formed in the first heat exchange cavity 013 to realize heat exchange between the mixing channel 014 and the fluid therein, i.e., to realize heat dissipation between the mixing channel 014 and the fluid therein, and to ensure that the heat generated by the mixing and dissolving of the fluid in the mixing channel 014 is dissipated in time so that the fluid therein is in an appropriate temperature range.
[0110] In particular, the volume ratio of the first heat exchange cavity 013 to the mixing channel 014 is 2 to 50, and preferably, the volume ratio of the first heat exchange cavity 013 to the mixing channel 014 is 5 to 30. Because the volume of the first heat exchange cavity 013 is larger than the volume of the mixing channel 014, the heat generated by the mixing and dissolving of the first group of reaction streams and the second group of reaction streams is conducted out in time.
[0111] Furthermore, a transition region 020 is provided between the mixing region 008 and the reaction region 009, and the transition region 020 includes a stabilization channel 021 having a constant cross-section and a diffusion channel 022 having a gradually expanding cross-section and arranged along a first direction and communicating with each other, the stabilization channel 021 communicating with the mixing channel 014, and the diffusion channel 022 communicating with the reaction region 009. The transition region 020 can merge mixed fluids from multiple mixing channels 014 in the stabilization channel 021 together to achieve another uniform mixing, and then deliver the mixed fluid into the reaction region 009 via the diffusion channel 022. In particular, the transition region 020 includes the stabilization channel 021 and the diffusion channel 022, the stabilization channel 021 mainly realizing the merging and mixing of fluids, and the diffusion channel 022 being capable of diffusion, for example, having a bell-mouth shape that can distribute the mixed fluid to multiple reaction channels 010, as described below. The two ends of the transition region 020 are provided with partition plates having through holes so as to isolate them from the mixing region 008 (mainly the first heat exchange cavity 013) and the reaction region 009 (mainly the second heat exchange cavity 012), respectively, and are connected in parallel to each mixing channel 014 and reaction channel 010 through each through hole of each partition plate, and the diffusion channel 022 and the stabilization channel 021 can be pipe fittings provided between the two partition plates.
[0112] Furthermore, the stabilization channel 021 can be connected to a discharge pipe 018 extending outside the shell 003. As described above, the stabilization channel 021 has the functions of merging and mixing, and the discharge pipe 018 can discharge bubbles and streams accumulated in the stabilization channel 021 to avoid the effects of bubble accumulation on the uniformity of mixing and stream blockage. A valve can be installed in the discharge pipe 018, and the valve can be opened when bubbles or streams need to be discharged.
[0113] Furthermore, the diffusion channel 022 is provided with a diffusion plate having a mesh or slits. The diffusion plate may be substantially perpendicular to the first direction. The fluid in the diffusion channel 022 can flow through the mesh or slits on the diffusion plate, thereby dispersing the fluid and improving the uniformity of the mixed fluid.
[0114] Specifically, the reaction region 009 includes multiple parallel reaction channels 010 extending along a first direction and communicating with a mixing channel 014 via stabilization channels 021 and diffusion channels 022. The reaction channels 010 provide a reaction space for the mixed fluid and support the mixed fluid flow along the first direction to the next stage of the collection region 024, thereby allowing the mixed fluid to react while forming a stable plug flow within the reaction channels 010 and avoiding undesired products due to inconsistent residence time distribution. As described above, a transition region 020 may be provided between the reaction region 009 and the mixing region 008, and the multiple reaction channels 010 may communicate with the diffusion channel 022, thereby uniformly distributing the mixed fluid within the diffusion channel 022 to the multiple reaction channels 010. The number of reaction channels may be, for example, 2 to 10,000 channels, preferably 2 to 5,000 channels, and more preferably 2 to 500 channels. The reaction channels 010 may have at least one cross-section of a circular, rectangular, or triangular shape.
[0115] Furthermore, the reaction channel 010 includes a second mixing element 011, which includes a base strip 0004 extending along the first direction and tooth elements 0005 connected to the base strip 0004 and extending transversely to the base strip 0004. In the second mixing element 011, the base strip 0004 provides support for the tooth elements 0005, so that the tooth elements 0005 can be stably held within the reaction channel 010, and the tooth elements 0005 extend in a direction substantially transverse to the reaction channel 010, which can improve the degree of turbulence of the fluid within the reaction channel 010 and thereby improve the mixing uniformity between the reaction streams.
[0116] Furthermore, the tooth-like members 0005 may have one of the following shapes: triangular, arcuate, wavy, and spiral. The tooth-like members 0005 extend transversely to the reaction channel 010 and may have various shapes as long as they can achieve the effect of increasing the turbulence of the fluid.
[0117] Preferably, the tooth-like member 0005 is triangular, with one corner connected to the base strip 0004 on one side of the triangle that is closest to the base strip 0004, and the other corner 0.01 mm to 20 mm away from the base strip 0004. The tooth-like member 0005 may also be a triangular plate member, with only one corner connected to the base strip 0004.
[0118] Preferably, the reaction channel 010 is provided with a plurality of second mixing elements 011 (2 to 100 elements, preferably 2 to 50 elements, more preferably 10 to 30 elements) stacked at intervals, the plurality of second mixing elements 011 are stacked at intervals, and the tooth-like elements 0005 are also stacked at intervals correspondingly, and the tooth-like elements 0005 of different second mixing elements 011 are arranged alternately, so that the different second mixing elements 011 are arranged more irregularly, which can better improve the degree of turbulence of the fluid in the reaction channel 010.
[0119] Preferably, the cross section of the reaction channel 010 is rectangular, and the tooth-like members 0005 extend between a pair of opposing sides of the rectangle. Specifically, the reaction channel 010 includes four side walls, i.e., two pairs of opposing parallel side walls, the base strip 0004 is disposed on one side wall of the reaction channel 010, and the tooth-like members 0005 extend toward the other opposing side wall, so that the plurality of second mixing elements 011 can better accommodate the rectangular prism-shaped internal cavity structure of the reaction channel 010.
[0120] In particular, the reaction channel 010 is 1 mm 2 ~150mm 2and a length of 50 mm to 5000 mm, the shortest distance between the reaction channels 010 is 1 mm to 50 mm, the second mixing member 011 has a thickness of 0.1 mm to 3 mm, and the interval between adjacent tooth-like members 0005 is 1 mm to 50 mm.
[0121] Preferably, the reaction channels 010 have a length of 100 mm to 3000 mm, the minimum spacing between the reaction channels 010 is 3 mm to 30 mm, the second mixing element 011 has a thickness of 0.2 mm to 2 mm, and the spacing between adjacent tooth-like elements 0005 is 1.5 mm to 20 mm. The minimum spacing between the reaction channels 010 reflects the density of the reaction channels 010 in the reaction region 009. Preferably, in the second mixing element 011, the tooth-like elements 0005 are plate-like elements that may be flush with the base strip 0004, and the thickness of the second mixing element 011 is approximately the same as the thickness of the tooth-like elements 0005.
[0122] Furthermore, the reaction region 009 may include a second heat exchange cavity 012 disposed within the shell 003, the reaction channel 010 being disposed within the second heat exchange cavity 012, and the shell 003 including a second heat transfer medium inlet 006 and a second heat transfer medium outlet 007 communicating with the second heat exchange cavity 012. The second heat exchange cavity 012 may be primarily formed by the shell 003, with a second partition plate 025 between the reaction region 009 and the collection region 024 and a partition plate between the reaction region 009 and the transition region 020 at its two ends, respectively. A heat exchange medium may be introduced into the second heat exchange cavity 012 via the second heat exchange medium inlet 006 and the second heat exchange medium outlet 007 to realize the heat exchange process of the reaction channel 010 and avoid the production of undesired products, so as to ensure that the fluid in the reaction channel 010 reacts within an appropriate temperature range.
[0123] Furthermore, the first heat exchange cavity 013 and the second heat exchange cavity 012 may be connected in series to each other and arranged in one heat exchange circulation flow path, or may be arranged in parallel in one heat exchange circulation flow path, or may be arranged in two different heat exchange circulation flow paths, respectively.
[0124] In particular, the volume ratio of the second heat exchange cavity 012 to the reaction channel 010 is 2 to 50, and preferably the volume ratio of the second heat exchange cavity 012 to the reaction channel 010 is 5 to 30. The volume of the second heat exchange cavity 012 is larger than the volume of the reaction channel 010, so that the heat in the reaction channel 010 can be discharged in a timely manner to ensure that the reaction channel 010 is at an appropriate temperature.
[0125] A preferred microchannel reactor of the present invention can be used to synthesize poly-α-olefin synthetic oil, and the feed pipe 002 can be used to feed a liquid phase stream (continuous phase) (the mixed stream from the feed unit 1), and the fluid distribution pipe 017 can be used to feed a gas phase stream (dispersed phase) (BF3 catalyst separately fed from the feed unit 1). The liquid phase stream is used as the continuous phase to enter the feed region 023 of the microchannel reactor from the feed pipe 002, and the gas phase stream is used as the dispersed phase to enter the mixing channel 014 of the reactor from the fluid distribution pipe 017 and dissolve in the continuous phase through the fluid distributor 016. The mixed fluid that has completed the reaction in the reaction channel 010 enters the recovery region 024 and is finally discharged from the discharge pipe 001.
[0126] In the embodiments of the present invention, the preferred structural components or parameters are employed in using the preferred microchannel reactor without repetition of details unless otherwise indicated.
[0127] FIG. 7 is a schematic diagram of a comparative apparatus of the present invention, in which the apparatus comprises an input unit 1, a tubular reactor 2, and a post-treatment unit 3, which are connected in series, and the input unit 1 comprises a mixer 12 for the auxiliary feedstock and the olefin feedstock, and a pipeline for separately supplying the BF3 catalyst. [Example]
[0128] Example 1 In this example, the mass ratio of BF3 directly fed into the microchannel reactor to BF3 fed into the mixer for mixing was 60:40, and the stream obtained by mixing a part of the BF3 catalyst and all of the auxiliary feedstock was passed through the microchannel reactor, and the rest of the BF3 catalyst and all of the olefin feedstock were passed through the microchannel reactor separately (the above-mentioned configuration form 2 and feeding form 2 of the present invention).
[0129] The mixer's structure and parameters were as follows: the mixer was a cylindrical structure with an outer diameter of 10 cm and an inner diameter of 6 cm. The mixer had two inlets at the bottom and one outlet at the top. The mixer was equipped with a packing layer, which consisted of ceramic balls. The mixer had a heat exchange layer with a temperature of 0 to 100°C.
[0130] In this apparatus, the microchannel reactor used is the preferred microchannel reactor of the present invention as described above, and includes five reaction channels 010 arranged in parallel, each of which has a length of 20 mm. 2 The reactor had a rectangular cross section with a cross-sectional area of 1000 mm, and the reaction channel 010 had a length of 2000 mm. The second mixing element 011 in the reaction channel 010 had triangular teeth 0005, and the spacing between adjacent teeth 0005 was 5 mm. A total of four layers of second mixing elements 011 were arranged in the reaction channel 010, stacked one on top of the other, as shown in Figure 5. The reactor had a diameter of 10 cm. 2 The fluid distributor 016 contained two mixing channels 014 with an average pore size of 5 microns and a cross-sectional area of 8.5 cm. 2 The mixing channel 014 was a sintered metal powder compact having a length of 150 mm. Three first mixing members 015 were provided in each mixing channel 014.
[0131] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0132] BF3 gas at a flow rate of 126 L / h and n-butanol at a rate of 0.6 L / h were mixed in a mixer. Microchannel reactor 2 was separately fed with the 1.2 L / h stream from the mixer, an additional 189 L / h of BF3 gas, and 60 L / h of decene. The polymerization reaction took place at a temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali wash and water wash for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 1.
[0133] [Table 1]
[0134] Example 2 In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40, a stream obtained by mixing a part of the BF3 catalyst with a part of the auxiliary material was passed through the microchannel reactor, and the rest of the BF3 catalyst, the rest of the auxiliary material, and the whole of the olefin raw material were each passed through the microchannel reactor separately (the above-mentioned Configuration Form 3 and Supply Form 3 of the present invention).
[0135] The mixer and microchannel reactor were of the same construction as those in Example 1.
[0136] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0137] BF3 gas at a flow rate of 126 L / h and n-butanol at 0.3 L / h were mixed in a mixer. Microchannel reactor 2 was separately fed with the 1.2 L / h flow from the mixer, 189 L / h of BF3 gas, 0.3 L / h of n-butanol, and 60 L / h of decene. The polymerization reaction took place at a temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali wash and water wash for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 2.
[0138] [Table 2]
[0139] Example 3 In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40, and a stream obtained by mixing a part of the BF3 catalyst, a part of the auxiliary material, and the whole of the olefin raw material was passed through the microchannel reactor, and the remaining BF3 catalyst and the remaining auxiliary material were passed through the microchannel reactor separately (the above-mentioned Configuration Form 4 and Supply Form 4 of the present invention).
[0140] Polymerization of the olefin raw material was carried out using the poly-α-olefin production apparatus shown in Figure 1.
[0141] In this device, the structure and parameters of the mixer 11 were as follows: the mixer was a cylindrical structure with an outer diameter of 10 cm and an inner diameter of 6 cm. The mixer had two inlets at the bottom end and one outlet at the top end. The mixer was equipped with a packing layer, and the packing was ceramic balls. The mixer had a heat exchange layer with a temperature of 0 to 100°C.
[0142] In this apparatus, the structure and parameters of the mixer 12 were as follows: the mixer was a cylindrical structure with an outer diameter of 10 cm and an inner diameter of 6 cm. The mixer had two inlets at the bottom end and one outlet at the top end. The mixer was equipped with a packing layer, and the packing material was a conventional packing material. The mixer had a heat exchange layer with a temperature of 0 to 50°C.
[0143] The microchannel reactor had the same structure as that in Example 1.
[0144] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0145] BF3 gas at a flow rate of 126 L / h and n-butanol at a flow rate of 0.3 L / h were mixed in mixer 11, and then the mixture was mixed with decene at a flow rate of 60 L / h in mixer 12. Microchannel reactor 2 was separately fed with a flow rate of 60.6 L / h through mixer 12, an additional independently supplied BF3 gas at a flow rate of 189 L / h, and n-butanol at a flow rate of 0.3 L / h. The polymerization reaction took place at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali scrubber and a water scrubber for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 3.
[0146] [Table 3]
[0147] Example 4 In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40, and a stream obtained by mixing a part of the BF3 catalyst, all of the auxiliary materials, and a part of the olefin raw material was passed through the microchannel reactor, and the rest of the BF3 catalyst and the rest of the olefin raw material were passed through the microchannel reactor separately (the above-mentioned Configuration Form 5 and Supply Form 5 of the present invention).
[0148] Polymerization of the olefin raw material was carried out using the poly-α-olefin production apparatus shown in Figure 1.
[0149] The mixer and microchannel reactor were of the same construction as those in Example 3.
[0150] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and the tank was filled with potassium oxide.
[0151] BF3 gas at a flow rate of 126 L / h and n-butanol at 0.6 L / h were mixed in mixer 11, and then the mixture was mixed with decene at a flow rate of 30 L / h in mixer 12. Microchannel reactor 2 was separately fed with a 30.6 L / h flow from mixer 12, an additional 189 L / h of BF3 gas, and 0.3 L / h of decene. The polymerization reaction took place at a temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali wash and water wash for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 4.
[0152] [Table 4]
[0153] Example 5 In this example, the mass ratio of BF3 directly fed into the microchannel reactor to BF3 fed into the mixer to participate in the mixing was 60:40, and the stream obtained by mixing a part of the BF3 catalyst, all of the auxiliary materials, and all of the olefin raw material was passed through the microchannel reactor, and the rest of the BF3 catalyst was passed through the microchannel reactor (the above-mentioned Configuration Form 6 and Supply Form 6 of the present invention).
[0154] The mixer and microchannel reactor were of the same construction as in Example 1, except that the mixer used had three feed ports.
[0155] The mixer and microchannel reactor were of the same construction as those in Example 3.
[0156] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0157] Mixing was carried out by passing BF3 gas at a flow rate of 126 L / h, n-butanol at 0.6 L / h, and decene at a flow rate of 60 L / h through the mixer. Microchannel reactor 2 was separately supplied with the flow from the mixer at a flow rate of 61.2 L / h and an additional, independently supplied BF3 gas at a flow rate of 189 L / h. The polymerization reaction took place at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali washing device and a water washing device for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 5.
[0158] [Table 5]
[0159] Example 6 In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer for mixing was 60:40. In the feeding unit, a part of the BF3 catalyst and all of the auxiliary feedstock were subjected to a first mixing, then to a second mixing with all of the olefin feedstock, and then the mixed stream was passed through the microchannel reactor, and the remaining BF3 catalyst was passed through the microchannel reactor separately (the above-mentioned Configuration Form 6 and Supply Form 6 of the present invention).
[0160] Polymerization of the olefin raw material was carried out using the poly-α-olefin production apparatus shown in FIG.
[0161] The mixer and microchannel reactor were of the same construction as those in Example 3.
[0162] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0163] BF3 gas at a flow rate of 126 L / h and n-butanol at a rate of 0.6 L / h were mixed in mixer 11, and the mixed stream and decene at a flow rate of 60 L / h were fed into mixer 12. Microchannel reactor 2 was separately fed with the stream from mixer 12 at a flow rate of 61.2 L / h and an additional, independently supplied BF3 gas at a flow rate of 189 L / h. The polymerization reaction took place at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali scrubber and a water scrubber for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 6.
[0164] [Table 6]
[0165] Example 7 In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer for mixing was 50:50. In the feeding unit, a part of the BF3 catalyst and all of the auxiliary feedstock were subjected to a first mixing, then to a second mixing with all of the olefin feedstock, and then the mixed stream was passed through the microchannel reactor, and the rest of the BF3 catalyst was passed through the microchannel reactor separately.
[0166] Polymerization of the olefin raw material was carried out using the poly-α-olefin production apparatus shown in FIG.
[0167] The mixer and microchannel reactor were of the same construction as those in Example 3.
[0168] In this device, the post-treatment unit 3 was a solid adsorption device, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom supply, top discharge, and tank filled with potassium oxide.
[0169] BF3 gas at a flow rate of 126 L / h and n-butanol at 0.6 L / h were mixed in mixer 11, and the mixed stream and decene at a flow rate of 60 L / h were fed into mixer 12. Microchannel reactor 2 was separately fed with the stream from mixer 12 at a flow rate of 61.2 L / h and an additional, independently supplied BF3 gas at a flow rate of 126 L / h. The polymerization reaction took place at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was then sent to an alkali wash and water wash for post-treatment. The catalyst was removed, yielding a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 7.
[0170] [Table 7]
[0171] Comparative Example 1 Olefin polymerization was carried out using the poly-α-olefin production apparatus shown in Figure 2. In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40, and a part of the BF3 catalyst and all of the auxiliary materials were subjected to a first mixing, then to a second mixing with all of the olefin material, and then the mixed flow was passed through the microchannel reactor, and the remaining BF3 catalyst was passed through the microchannel reactor separately.
[0172] The mixer had the same construction as that of Example 3.
[0173] In this device, the microchannel reactor 2 contains five reaction channels 010 in parallel, each of which has a diameter of 20 mm. 2 The reactor 010 had a rectangular cross-section with a cross-sectional area of 1000 mm, and the reaction channel 010 had a length of 2000 mm. The second mixing element 011 in the reaction channel 010 had triangular teeth 0005, and the spacing between adjacent teeth 0005 was 5 millimeters. A total of four layers of second mixing elements 011 were arranged on top of each other in the reaction channel 010, as shown in Figure 5. Neither a mixing channel 014 nor a fluid distributor 016 was present in the reactor.
[0174] In this device, the post-treatment unit 3 was an adsorption unit, and its structure and parameters were as follows: open type, effective volume 10 L, normal temperature operation, bottom feed, top discharge, adsorption device filled with calcium oxide.
[0175] BF3 gas at a flow rate of 126 L / h and n-butanol at a rate of 0.6 L / h were mixed in mixer 11, and the mixed stream and decene at a flow rate of 60 L / h were fed into mixer 12. Microchannel reactor 2 was separately fed with the stream from mixer 12 at a flow rate of 61.2 L / h and an additional, independently supplied BF3 gas at a flow rate of 189 L / h. Polymerization occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was fed into an adsorption device to remove the catalyst by adsorption, producing a polyolefin product. A small sample was taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 8.
[0176] [Table 8]
[0177] Comparative Example 2 A polymerization reaction was carried out using the poly-α-olefin production apparatus shown in Figure 2. In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40, and a part of the BF3 catalyst and all of the auxiliary materials were subjected to a first mixing, then to a second mixing with all of the olefin material, and then the mixed flow was passed through the microchannel reactor, and the remaining BF3 catalyst was passed through the microchannel reactor separately.
[0178] The microchannel reactor had the same structure as that in Example 3.
[0179] In this device, the microchannel reactor 2 contains five reaction channels 010 in parallel, each of which has a diameter of 20 mm. 2The reactor had a rectangular cross section with a cross-sectional area of 1000 mm, and the reaction channel 010 had a length of 2000 mm. The second mixing element 011 in the reaction channel 010 had triangular teeth 0005, and the spacing between adjacent teeth 0005 was 5 mm. A total of four layers of second mixing elements 011 were arranged in the reaction channel 010, stacked one on top of the other, as shown in Figure 5. The reactor had a diameter of 10 cm. 2 The fluid distributor 016 contained one mixing channel 014 with an average pore size of 5 microns and a cross-sectional area of 8.5 cm. 2 The mixing channel 014 was a sintered metal powder compact having a length of 150 mm. Three first mixing members 015 were provided in the mixing channel 014.
[0180] In this device, the post-treatment unit 3 was a centrifugal separator, the structure and parameters of which were as follows: tube-type centrifuge, room temperature operation, and a separation factor of 8000G.
[0181] BF3 gas at a flow rate of 126 L / h and n-butanol at a rate of 0.6 L / h were mixed in mixer 11, and the mixed stream and decene at a flow rate of 60 L / h were fed into mixer 12. Microchannel reactor 2 was separately fed with the 61.2 L / h stream from mixer 12 and an additional 189 L / h of BF3 gas. Polymerization occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was centrifuged to remove the catalyst and washed three times with water to produce a polyolefin product. After the system reached stable operation, a small sample was taken and the contents of each component in the product were determined by gas chromatography. The test results are shown in Table 9.
[0182] [Table 9]
[0183] Example 8 Polymerization of an olefin feedstock was carried out using the poly-α-olefin production apparatus shown in Figure 2. In this example, the mass ratio of BF3 directly fed to the microchannel reactor to BF3 fed to the mixer to participate in the mixing was 60:40. In the feeding unit, a portion of the BF3 catalyst and all of the auxiliary materials were subjected to a first mixing, then to a second mixing with all of the olefin feedstock, and then the mixed flow was passed through the microchannel reactor, and the remaining BF3 catalyst was passed through the microchannel reactor separately.
[0184] The mixer and microchannel reactor were of the same construction as those in Example 3. In this device, the microchannel reactor 2 contains five reaction channels 010 in parallel, each of which has a diameter of 20 mm. 2 The reactor had a rectangular cross section with a cross-sectional area of 1000 mm, and the reaction channel 010 had a length of 2000 mm. The second mixing element 011 in the reaction channel 010 had triangular teeth 0005, and the spacing between adjacent teeth 0005 was 5 mm. A total of four layers of second mixing elements 011 were arranged in the reaction channel 010, stacked one on top of the other, as shown in Figure 5. The reactor had a diameter of 10 cm. 2 The fluid distributor 016 included two mixing channels 014 having a cross-sectional area of 8.5 cm and a length of 800 mm. Three first mixing elements 015 were provided in each mixing channel 014. The fluid distributor 016 was made of micro / mesoporous tubular material, and the hollow microchannels constituting the network of the micro / mesoporous tubular material were 8.5 cm in length. 2 The microporous membrane had a cross-sectional area of 1.0 mm, an average pore size of 2 microns, and a length of 150 mm.
[0185] In this device, the post-treatment unit 3 was a centrifugal separator, the structure and parameters of which were as follows: tube-type centrifuge, room temperature operation, and a separation factor of 8000G.
[0186] BF3 gas at a flow rate of 126 L / h and n-butanol at 0.6 L / h were mixed in mixer 11, and the mixed stream and decene at a flow rate of 60 L / h were fed into mixer 12. Microchannel reactor 2 was fed with BF3 gas at a flow rate of 61.2 L / h through mixer 12 and an additional, independently supplied BF3 gas at a flow rate of 189 L / h. Polymerization occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was centrifuged to remove the catalyst and washed three times with water to produce a polyolefin product. After the system was operating stably, a small sample was taken and the contents of each component in the product were determined by gas chromatography. The test results are shown in Table 10.
[0187] [Table 10]
[0188] Comparative Example 3 In this example, the structure and parameters of the microchannel reactor 2 were the same as those in Example 1.
[0189] In this device, the post-treatment unit 3 is an adsorption device, and its structure and parameter process are as follows: open type, effective volume 10 L, normal temperature operation, bottom feed, top discharge, adsorption device filled with calcium oxide.
[0190] Microchannel reactor 2 was independently fed with BF3 gas at a flow rate of 315 L / h, n-butanol at a flow rate of 0.6 L / h, and decene at a flow rate of 60 L / h. The polymerization reaction occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was fed to an adsorption device to remove the catalyst by adsorption and produce a polyolefin product. After the system was operating stably, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 11.
[0191] [Table 11]
[0192] Comparative Example 4 In this example, the structures and parameters of the mixer and the microchannel reactor 2 were the same as those in Example 1.
[0193] In this device, the post-treatment unit 3 is an adsorption device, and its structure and parameter process are as follows: open type, effective volume 10 L, normal temperature operation, bottom end feeding, top end discharging, adsorption device filled with calcium oxide.
[0194] BF3 gas at a flow rate of 315 L / h and n-butanol at a rate of 0.6 L / h were mixed in a mixer. The mixed stream and decene at a flow rate of 60 L / h were independently fed into microchannel reactor 2. The polymerization reaction occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was fed into an adsorption device to remove the catalyst by adsorption and produce a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 12.
[0195] [Table 12]
[0196] Comparative Example 5 In this example, the structures and parameters of the mixer and the microchannel reactor 2 were the same as those in Example 1.
[0197] In this device, the post-treatment unit 3 is an adsorption device, and its structure and parameter process are as follows: open type, effective volume 10 L, normal temperature operation, bottom end feeding, top end discharging, adsorption device filled with calcium oxide.
[0198] 0.6 L / h of n-butanol and 60 L / h of decene were mixed in a mixer. The mixed stream at a flow rate of 61.2 L / h and BF3 gas at a flow rate of 315 L / h were independently fed into microchannel reactor 2. The polymerization reaction occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was fed into an adsorption device to remove the catalyst by adsorption and produce a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 13.
[0199] [Table 13]
[0200] Comparative Example 6 The polymerization of the olefin raw material was carried out using the poly-α-olefin production apparatus shown in FIG.
[0201] In this apparatus, the mixer had the same structure and parameters as in Example 1.
[0202] In this apparatus, the tubular reactor included a reaction tube and a hollow cylindrical shell containing a heat exchange medium, and the reaction tube was spirally arranged within the hollow cylindrical shell. Baffle plates were arranged at intervals along the circumferential direction within the hollow cylindrical shell, and the baffle plates extended along the cross-sectional direction of the reaction tube and had through-holes capable of accommodating the reaction tube, allowing the reaction tube to pass through the baffle plates. The cylindrical shell was provided with a heat exchange medium inlet and a heat exchange medium outlet.
[0203] In this example, the post-treatment unit 3 was an adsorption device, which had the same structure and process parameters as those in Example 3.
[0204] 0.6 L / h of n-butanol and 60 L / h of decene were mixed in a mixer. The mixed stream at a flow rate of 61.2 L / h and BF3 gas at a flow rate of 315 L / h were independently fed into microchannel reactor 2. The polymerization reaction occurred in microchannel reactor 2 at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was fed into an adsorption device to remove the catalyst by adsorption and produce a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 14.
[0205] [Table 14]
[0206] Comparative Example 7 In this example, the structures and parameters of the mixer and the microchannel reactor 2 were the same as those in Example 1.
[0207] BF3 gas at a flow rate of 5 L / h and n-butanol at a flow rate of 0.6 L / h were mixed in a mixer, and the mixed stream was passed through microchannel reactor 2. 1-Decene was also passed through microchannel reactor 2 at a flow rate of 30 L / h. The polymerization reaction occurred in the microchannel reactor at a reaction temperature of 20°C and a pressure of 5 MPa. The resulting stream was then fed into an adsorption device to remove the catalyst by adsorption and produce a polyolefin product. After the system reached stable operation, samples were taken and the contents of each component in the product were measured by gas chromatography. The test results are shown in Table 15.
[0208] [Table 15]
[0209] The polyolefin products of Examples 1 to 8 and Comparative Examples 1 to 7 were each distilled and cut to obtain poly-α-olefin synthetic oils above 280°C, and the kinematic viscosity and viscosity index at 100°C were tested. The test results are shown in Table 16.
[0210] [Table 16]
[0211] The above examples and comparative examples show that the specific method for producing poly-α-olefin synthetic oil of the present invention can improve the conversion rate of the target product. Furthermore, by using a preferred microchannel reactor, the method for synthesizing poly-α-olefin synthetic oil achieved a high conversion rate. This is because the reaction channel 010 and the mixing channel 014 have a tubular structure arranged in the same direction, allowing the mixed fluid to form a stable plug flow along the first direction, improving the consistency of the mixed fluid residence time and preventing or reducing the production of undesired products. In addition, the reaction channel 10 is equipped with a second mixing element 011, and the mixing channel 014 is equipped with a fluid distributor 016 and a first mixing element 015, which further improves the turbulence of the mixed fluid, improving the uniformity of mixing, and further preventing or reducing the production of undesired products, thereby improving the conversion rate of the target product.
[0212] Furthermore, it can be seen from the above Examples and Comparative Examples that by using the method for producing poly-α-olefin synthetic oil of the present invention, it is possible to obtain poly-α-olefin synthetic oil that is excellent in both kinematic viscosity and viscosity index.
[0213] Although the preferred embodiments of the present invention have been described in detail above with reference to the drawings, the present invention is not limited thereto. Within the technical spirit of the present invention, various simple modifications, including combinations of various specific technical features in any suitable manner, may be made to the technical solutions of the present invention. To avoid unnecessary repetition, various possible combinations will not be described in detail in this specification. However, these simple modifications and combinations should be considered as the disclosure of the present invention, and all fall within the protection scope of the present invention.
Claims
1. The feed unit (1), the microchannel reactor (2), and the post-treatment unit (3) are connected in series, and the feed unit is a mixer and / or a reactor for feeding an olefin feedstock, an auxiliary feedstock, and BF 3 a pipeline for delivering a catalyst to said microchannel reactor (2); The input unit (1) is configured to add at least a part of the auxiliary material and the BF 3 a mixer for mixing at least a portion of the catalyst; 3 and a pipeline for individually supplying at least a portion of the catalyst to the microchannel reactor (2), The microchannel reactor (2) comprises: A shell (003), in which a supply region (023), a mixing region (008), a reaction region (009) and a collection region (024) are successively arranged in a first direction within the shell (003) and communicate with each other, wherein a transition region is provided between the mixing region and the reaction region, and the transition region comprises a stabilization channel having a constant cross section and a diffusion channel having a gradually expanding cross section, the stabilization channel being arranged in the first direction and communicating with each other, and the diffusion channel is in communication with the reaction zone, wherein the shell (003) is provided with a supply pipe (002) in communication with the supply zone (023) and a discharge pipe (001) in communication with the collection zone (024), the mixing zone (008) is provided with a mixing channel (014) extending along the first direction, and the reaction zone comprises 2 to 10,000 reaction channels extending along the first direction and in communication with the mixing channel through the transition zone; a fluid distribution pipe (017) extending from the exterior of the shell (003) into the mixing channel (014), the fluid distribution pipe (017) being connected to a fluid distributor (016) at an end of the mixing channel (014); The supply pipe (002) is used to feed the raw material from the feeding unit, and the fluid distribution pipe (017) is used to feed the BF of the feeding unit (1). 3 connected to the pipeline for separate supply of catalyst, BF 3 can be used to charge a catalyst, The discharge pipe (001) is connected to a post-treatment unit (3), The fluid distributor (016) is at least one selected from a powder sintered body having micropores, a mesoporous foam material, a wire mesh, and a tube having microslits or micropores; the mixing area (008) comprises 2 to 100 mixing channels (014), and the fluid distribution pipes (017) include a main pipe extending from the outside of the shell to the supply area, and a distribution pipe extending from the supply area to each mixing channel with a fluid distributor connected to the end of the distribution pipe; In the mixing channel (014), a first mixing element is disposed downstream of the fluid distributor; and the first mixing element includes a main flow section and a branch flow section that are alternately arranged and communicate with each other along the first direction, the main flow section including a single main flow path, and the branch flow section including a plurality of branch flow paths; and a collection cavity communicating with the plurality of diversion channels is disposed downstream of the diversion section; An apparatus for producing polyalphaolefins, wherein the secondary feedstock is one or more alcohols having 1 to 20 carbon atoms.
2. The feeding unit (1) 3 a mixer for mixing a portion of the catalyst, a portion of the auxiliary material, and a portion of the olefin raw material; 3 a pipeline for passing the remainder of the catalyst, the remainder of the auxiliary feedstock, and the remainder of the olefin feedstock separately into the microchannel reactor (2) based on the type of feedstock; or The feeding unit (1) 3 a mixer for mixing a part of the catalyst and all of the auxiliary materials; 3 a pipeline for separately passing the remainder of the catalyst through the microchannel reactor (2) and a pipeline for separately passing the entire olefin feedstock through the microchannel reactor (2); or The feeding unit (1) 3 a mixer for mixing a portion of the catalyst and a portion of the auxiliary material; 3 a pipeline for passing the remainder of the catalyst, the remainder of the auxiliary feedstock, and the entire olefin feedstock separately through the microchannel reactor (2); or The feeding unit (1) 3 a mixer for mixing a part of the catalyst, a part of the auxiliary material, and the whole of the olefin raw material; 3 a pipeline for passing the remainder of the catalyst and the remainder of the auxiliary material separately through said microchannel reactor (2); or The feeding unit (1) 3 a mixer for mixing a part of the catalyst, all of the auxiliary materials, and a part of the olefin raw material; 3 a pipeline for passing the remainder of the catalyst and the remainder of the olefin feedstock separately through the microchannel reactor (2); or The feeding unit (1) 3 a mixer for mixing a part of the catalyst, all of the auxiliary materials, and all of the olefin raw material; 3 a pipeline for passing the remainder of the catalyst separately through the microchannel reactor (2); The BF 3 2. The apparatus according to claim 1, wherein when the catalyst, the auxiliary material, and the olefin feedstock are mixed in the feeding unit, the feeding unit comprises a first mixer for mixing any two of the three feedstocks and a second mixer for mixing the mixture from the first mixer and the remaining one feedstock, wherein the first mixer is in communication with the second mixer, and the second mixer is in communication with the microchannel reactor (2).
3. The fluid distributor is a cylindrical powder sintered body having micropores, and the fluid distributor has a diameter of 0.01 cm. 2 ~200cm 2 and a length of 1 mm to 2000 mm; and / or The mixing region (008) comprises 2 to 10 mixing channels (014), the mixing channels having a circular cross section; and the mixing channels have a diameter of 0.05 cm. 2 ~400cm 2 and a length of 50 mm to 5000 mm; and / or the mixing region includes a first heat exchange cavity within the shell, the mixing channel is disposed within the first heat exchange cavity, the shell includes a first heat exchange medium inlet and a first heat exchange medium outlet in communication with the first heat exchange cavity, and a volume ratio of the first heat exchange cavity to the mixing channel is between 2 and 50; and / or a discharge pipe extending outside the shell is connected to the stabilization channel; and / or the diffusion channel comprises a diffusion plate having a mesh or slits; and / or the reaction channel comprises a second mixing element, the second mixing element including a base strip extending along the first direction and tooth members connected to the base strip and extending transversely relative to the base strip, the tooth members being at least one of triangular, arcuate, wavy, and spiral; and / or Each reaction channel independently comprises a plurality of spaced apart second mixing elements, with the teeth of the second mixing elements being staggered; and / or the reaction channel has a cross section of at least one of a circle, a rectangle, and a triangle; and / or The reaction channel is 1 mm 2 ~150mm 2 and a length of 50 mm to 5000 mm, the shortest distance between the reaction channels is 1 mm to 50 mm, the second mixing element has a thickness of 0.1 mm to 3 mm, and the spacing between adjacent tooth elements is 1 mm to 50 mm; and / or 2. The apparatus of claim 1, wherein the reaction zone comprises a second heat exchange cavity disposed within the shell, the reaction channel is disposed within the second heat exchange cavity, the shell comprises a second heat exchange medium inlet and a second heat exchange medium outlet communicating with the second heat exchange cavity, and a volume ratio of the second heat exchange cavity to the reaction channel is 2 to 50.
4. 4. The apparatus according to any one of claims 1 to 3, characterized in that the post-treatment unit (3) allows the stream entering therein to be subjected to post-treatment to produce a polyolefin product, the post-treatment unit (3) being one or more of an adsorption unit, an extraction unit, a distillation unit, a centrifuge unit, a precipitation unit, an alkaline wash unit, and a water wash unit.
5. The BF in the microchannel reactor (2) 3 The BF directly fed to the microchannel reactor (2) is based on the total mass of 3 The BF mixed with the catalyst in the dosing unit 3 5. The apparatus according to claim 1, wherein the mass ratio of the catalyst to the catalyst is 90-10:10-90.
6. the reaction region comprises 2 to 500 channels extending along the first direction and communicating with the mixing channel through the transition region; and / or the reaction channel comprises a second mixing element, the second mixing element comprising a base strip extending along the first direction, and a tooth-like element connected to the base strip and extending transversely to the base strip, the tooth-like element being triangular, one side of the triangle being adjacent to the base strip, one end being connected to the base strip, and the other end being 0.01 mm to 20 mm away from the base strip; and / or the reaction channel has a rectangular cross section, and the teeth extend between opposing pairs of the rectangular cross sections; and / or The reaction channels have a length of 100 mm to 3000 mm, the shortest distance between the reaction channels is 3 mm to 30 mm, the second mixing element has a thickness of 0.2 mm to 2 mm, and the spacing between adjacent teeth is 1.5 mm to 20 mm; and / or The BF in the microchannel reactor (2) 3 The BF directly fed to the microchannel reactor (2) is based on the total mass of 3 The BF mixed with the catalyst in the dosing unit 3 2. The apparatus according to claim 1, wherein the mass ratio of the catalyst to the catalyst is 70-50:30-50.
7. A method for producing a polyα-olefin by using the apparatus for producing a polyα-olefin according to any one of claims 1 to 6, comprising: BF through the input unit 3 and introducing a catalyst, an auxiliary material, and an olefin feedstock into a microchannel reactor, subjecting the catalyst, the auxiliary material, and the olefin feedstock to a polymerization reaction in the microchannel reactor, followed by post-processing to produce a polyolefin product, wherein at least a portion of the auxiliary material and the BF 3 At least a portion of the catalyst is mixed in the dosing unit, and simultaneously, the BF 3 At least a portion of the catalyst is separately fed to the microchannel reactor, and in the microchannel reactor, the auxiliary feedstock, the olefin feedstock and the total amount of BF 3 The mass ratio of the catalyst is 1:1 to 1000:1 to 500; The BF in the microchannel reactor 3 The BF is individually fed to the microchannel reactor based on the total mass of 3 The catalyst and the BF are mixed in the dosing unit. 3 The mass ratio to the catalyst is 90 to 10:10 to 90, A method for producing poly-α-olefins, wherein the auxiliary raw material is one or more alcohols having 1 to 20 carbon atoms.
8. In the feeding unit, the BF 3 A portion of the catalyst, a portion of the auxiliary feedstock, and a portion of the olefin feedstock are mixed and then passed through the microchannel reactor, with the remaining BF being added based on the type of feedstock. 3 The catalyst, the remaining auxiliary feedstock and the remaining olefin feedstock are passed separately through the microchannel reactor; or In the feeding unit, the BF 3 A stream obtained by mixing a portion of the catalyst and all of the auxiliary materials is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and all of the olefin feedstock are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst and all of the auxiliary materials are mixed in a mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 100,000 L / h, the rate at which all of the auxiliary materials supplied to the mixer pass through the mixer is 0.01 to 1,000 L / h, and the BF 3 The rate at which the mixture obtained after mixing a portion of the catalyst and all of the auxiliary materials in the mixer passes through the microchannel reactor is 0.01 to 2000 L / h, and the BF 3 The rate at which the remainder of the catalyst is individually passed through the microchannel reactor is 1 to 150,000 L / h, and the rate at which the entire olefin feedstock is individually passed through the microchannel reactor is 10 to 5,000 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst and a portion of the auxiliary material is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst, the remainder of the auxiliary feedstock, and all of the olefin feedstock are each individually passed through the microchannel reactor, and the BF 3 When a part of the catalyst and a part of the auxiliary material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 100,000 L / h, the rate at which a portion of the auxiliary material passes through the mixer is 0.01 to 800 L / h, and the BF 3 The rate at which the mixture obtained by mixing a portion of the catalyst and a portion of the auxiliary material in the mixer passes through the microchannel reactor is 0.01 to 1600 L / h, and the BF 3 The remaining catalyst is passed through the microchannel reactor at a rate of 1 to 120,000 L / h, the remaining auxiliary material is passed through the mixer at a rate of 0.01 to 200 L / h, and the entire olefin feedstock is passed through the microchannel reactor at a rate of 10 to 5,000 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, a portion of the auxiliary feedstock, and all of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and the remainder of the auxiliary material are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, a part of the auxiliary material, and the whole of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 100,000 L / h, the rate at which a portion of the auxiliary feedstock passes through the mixer is 0.01 to 800 L / h, and the rate at which the entire olefin feedstock passes through the mixer is 10 to 5,000 L / h; 3 The mixture obtained by mixing a part of the catalyst, a part of the auxiliary material, and the whole of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 0.01 to 6000 L / h, and the BF 3 The remaining catalyst flows through the microchannel reactor at a rate of 1 to 150,000 L / h, and the remaining auxiliary materials flow through the microchannel reactor at a rate of 0.01 to 200 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, all of the auxiliary feedstock, and a portion of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and the remainder of the olefin feedstock are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, all of the auxiliary materials, and a part of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 100,000 L / h, the rate at which all of the auxiliary feedstock passes through the mixer is 0.01 to 1,000 L / h, and the rate at which a portion of the olefin feedstock passes through the mixer is 1 to 2,000 L / h; 3 The mixture obtained by mixing a part of the catalyst, all of the auxiliary materials, and a part of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 0.01 to 3000 L / h, and the BF 3 The remaining catalyst is individually passed through the microchannel reactor at a rate of 1 to 150,000 L / h, and the remaining olefin feedstock is individually passed through the microchannel reactor at a rate of 9 to 3,000 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, all of the auxiliary feedstock, and all of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst is passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, all of the auxiliary materials, and all of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 100,000 L / h, the rate at which all of the auxiliary feedstock passes through the mixer is 0.01 to 1,000 L / h, and the rate at which all of the olefin feedstock passes through the mixer is 10 to 5,000 L / h; 3 The mixture obtained by mixing a part of the catalyst, all of the auxiliary materials, and all of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 10 to 6000 L / h, and the BF 3 8. The method according to claim 7, wherein the rate at which the remainder of the catalyst passes through each of the microchannel reactors is 1 to 150,000 L / h.
9. The olefin in the olefin feedstock is C 3 ~C 20 α-olefins; optionally, the olefin feedstock is one or more of 5 ~C 20 Alkanes and / or C 1 ~C 20 8. The method of claim 7 further comprising a mixture of oxygen-containing compounds.
10. The method according to any one of claims 7 to 9, wherein the reaction temperature in the microchannel reactor is 0 to 120°C, the reaction pressure in the microchannel reactor is 0.01 to 10 MPa, and the residence time of the olefin feedstock in the microchannel reactor is 1 to 3600 seconds.
11. The BF in the microchannel reactor 3 The BF is individually fed to the microchannel reactor based on the total mass of 3 The catalyst and the BF are mixed in the dosing unit. 3 The method according to any one of claims 7 to 10, characterized in that the mass ratio of the catalyst to the catalyst is 80-40:20-60.
12. the post-treatment method is one or more of an adsorption method, a centrifugation method, a sedimentation method, an alkali washing method, a water washing method, and a gas-liquid separation method; 12. The method according to any one of claims 7 to 11, wherein when the post-treatment method is a sedimentation method or a centrifugation method, optionally, the obtained heavy liquid phase is returned to the dosing unit or the microchannel reactor to continue to participate in the continuous reaction.
13. The method according to any one of claims 7 to 12, wherein a poly-α-olefin is produced by utilizing the apparatus for producing a poly-α-olefin according to any one of claims 1 to 6.
14. In the feeding unit, the BF 3 A stream obtained by mixing a portion of the catalyst and all of the auxiliary materials is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and all of the olefin feedstock are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst and all of the auxiliary materials are mixed in a mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 30,000 L / h, the rate at which all of the auxiliary materials supplied to the mixer pass through the mixer is 0.2 to 500 L / h, and the BF 3 The rate at which the mixture obtained after mixing a portion of the catalyst and all of the auxiliary materials in the mixer passes through the microchannel reactor is 0.2 to 1000 L / h, and the BF 3 The rate at which the remainder of the catalyst is individually passed through the microchannel reactor is 10 to 50,000 L / h, and the rate at which the entire olefin feedstock is individually passed through the microchannel reactor is 40 to 2,500 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst and a portion of the auxiliary material is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst, the remainder of the auxiliary feedstock, and all of the olefin feedstock are each individually passed through the microchannel reactor, and the BF 3 When a part of the catalyst and a part of the auxiliary material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 30,000 L / h, the rate at which a portion of the auxiliary material passes through the mixer is 0.2 to 400 L / h, and the BF 3 The rate at which the mixture obtained by mixing a portion of the catalyst and a portion of the auxiliary material in the mixer passes through the microchannel reactor is 0.2 to 800 L / h, and the BF 3 The remaining catalyst is passed through the microchannel reactor at a rate of 10 to 40,000 L / h, the remaining auxiliary material is passed through the mixer at a rate of 0.2 to 100 L / h, and the entire olefin feedstock is passed through the microchannel reactor at a rate of 40 to 2,500 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, a portion of the auxiliary feedstock, and all of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and the remainder of the auxiliary material are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, a part of the auxiliary material, and the whole of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 30,000 L / h, the rate at which a portion of the auxiliary feedstock passes through the mixer is 0.2 to 400 L / h, and the rate at which the entire olefin feedstock passes through the mixer is 40 to 2,500 L / h; 3 The mixture obtained by mixing a part of the catalyst, a part of the auxiliary material, and the whole of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 0.2 to 3000 L / h, and the BF 3 The remaining catalyst flows through the microchannel reactor at a rate of 10 to 50,000 L / h, and the remaining auxiliary materials flow through the microchannel reactor at a rate of 0.2 to 100 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, all of the auxiliary feedstock, and a portion of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst and the remainder of the olefin feedstock are each passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, all of the auxiliary materials, and a part of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 30,000 L / h, the rate at which all of the auxiliary feedstock passes through the mixer is 0.2 to 500 L / h, and the rate at which a portion of the olefin feedstock passes through the mixer is 10 to 500 L / h; 3 The mixture obtained by mixing a part of the catalyst, all of the auxiliary materials, and a part of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 0.2 to 1000 L / h, and the BF 3 The remaining catalyst is individually passed through the microchannel reactor at a rate of 10 to 50,000 L / h, and the remaining olefin feedstock is individually passed through the microchannel reactor at a rate of 30 to 2,000 L / h; or In the feeding unit, the BF 3 The stream obtained by mixing a portion of the catalyst, all of the auxiliary feedstock, and all of the olefin feedstock is passed through the microchannel reactor, and the BF 3 The remainder of the catalyst is passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst, all of the auxiliary materials, and all of the olefin raw material are mixed in the mixer, the BF 3 The rate at which a portion of the catalyst passes through the mixer is 1 to 30,000 L / h, the rate at which all of the auxiliary feedstock passes through the mixer is 0.2 to 500 L / h, and the rate at which all of the olefin feedstock passes through the mixer is 40 to 2,500 L / h; 3 The mixture obtained by mixing a part of the catalyst, all of the auxiliary materials, and all of the olefin raw material in the mixer passes through the microchannel reactor at a rate of 0.2 to 3000 L / h, and the BF 3 8. The method according to claim 7, wherein the rate at which the remainder of the catalyst passes through each of the microchannel reactors is 10 to 50,000 L / h.
15. In the feeding unit, the BF 3 A portion of the catalyst and all of the auxiliary feedstock are subjected to a first mixing in a first mixer, and then subjected to a second mixing with all of the olefin feedstock in a second mixer, and the mixed stream is passed through the microchannel reactor, and then the BF 3 The remainder of the catalyst is passed separately through the microchannel reactor, and the BF 3 When a part of the catalyst and all of the auxiliary material are subjected to the first mixing in the first mixer, the BF 3 a rate at which a portion of the catalyst passes through the first mixer is 1 to 100,000 L / h, a rate at which all of the auxiliary materials pass through the first mixer is 0.01 to 1,000 L / h, and then the stream obtained after the first mixing is subjected to a second mixing with all of the olefin feedstock in the second mixer, a rate at which the stream obtained after the first mixing passes through the second mixer is 0.01 to 2,000 L / h, a rate at which all of the olefin feedstock passes through the second mixer is 10 to 5,000 L / h, and a rate at which the stream obtained after the second mixing passes through the microchannel reactor is 10 to 7,000 L / h; 3 The rate at which the remainder of the catalyst passes individually through the microchannel reactor is 1 to 150,000 L / h; and / or The reaction temperature in the microchannel reactor is 20 to 60°C, the reaction pressure in the microchannel reactor is 0.1 to 6 MPa, and the residence time of the olefin feedstock in the microchannel reactor is 15 to 1000 seconds; and / or The BF in the microchannel reactor 3 The BF is individually fed to the microchannel reactor based on the total mass of 3 The catalyst and the BF are mixed in the dosing unit. 3 The method according to claim 7, characterized in that the mass ratio of the catalyst to the catalyst is 70-50:30-50.
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