CN218012654U - Microchannel reactor - Google Patents
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- CN218012654U CN218012654U CN202221235004.4U CN202221235004U CN218012654U CN 218012654 U CN218012654 U CN 218012654U CN 202221235004 U CN202221235004 U CN 202221235004U CN 218012654 U CN218012654 U CN 218012654U
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Abstract
The utility model provides a microchannel reactor, includes at least one pre-mixing chamber (3), at least one mixing reaction chamber (6) and the reaction unit of order series connection, pre-mixing chamber be equipped with the first entry of pre-mixing chamber, pre-mixing chamber second entry, mixing reaction chamber still be equipped with the mixing chamber entry, the reaction unit constitute by distribution chamber (8), many parallelly connected reaction channel (9) and collection room (10) that communicate in proper order, the mixed reaction chamber export of end with distribution chamber communicate with each other, collection room (10) be equipped with export (11). The utility model provides a microchannel reactor passes through at least two-stage and mixes, has realized the one-time reaction of multiple material in same microchannel reactor, has reinforceed each stage simultaneously and has mixed the effect.
Description
Technical Field
The utility model relates to a reactor, specifically speaking relates to a microchannel reactor with can regulate and control heat transfer function.
Background
The microchannel reactor has the advantages of large specific surface area, good mixing and mass and heat transfer effects, accurate control of reaction time, accurate temperature control and the like due to small space characteristic size, and has great industrialization potential after being applied to various petrochemical systems.
The micro-reactor has strong advantages in mass transfer and heat exchange capacity, can better solve the reaction problem of a strong heat release or strong heat absorption system, and achieves the purpose of controlling the conversion rate and selectivity by better controlling the reaction temperature and quickly and efficiently mixing. During the synthesis reaction of poly-alpha-olefin, a gas-phase catalyst and a liquid-phase auxiliary agent are adopted, the gas-phase catalyst and the liquid-phase auxiliary agent are required to be completely mixed according to a certain proportion to have better catalysis effect, the gas-liquid phase mixture of the catalyst and the alpha-olefin start to react quickly after being mixed, and the heat release is very large and far greater than that in a reaction channel. The prior art does not take this into account, and the lack of heat removal capability at local locations is increasingly highlighted by the amplification of the microchannel reactor.
The disclosure of CN108786678A proposes a microreactor, comprising an upper layer, a middle layer and a lower layer, the upper layer being a heat exchange fluid inlet layer, the lower layer being a heat exchange fluid outlet layer, the upper layer and the lower layer being provided with heat exchange fluid channels; and an intermediate mixing layer separated by the heat exchange fluid channels into reactant fluid channels, the intermediate mixing layer having at least two fluid inlets for mixing the incoming fluids in the reactant fluid channels prior to discharge. On one hand, each layer plate of the plate-type microchannel reactor is provided with one or more limited channels, and certain limitation exists on amplification, and on the other hand, the technology is suitable for a system with relatively excessive heat transfer capacity and relatively uniform distribution of heat absorption and heat release in the channels.
CN208975763U discloses a multichannel microreactor, which comprises a distribution chamber, a reaction heat exchange zone and a collection chamber in sequence, wherein the distribution chamber is provided with a distribution member, the reaction heat exchange zone is composed of a plurality of reaction channels and adjacent heat exchange channels, the reaction channels are provided with a mixing member, and a heat exchange medium inlet is communicated with a heat exchange medium outlet through the heat exchange channels. In certain chemical reaction processes, due to the fact that reactant concentration at an inlet is high and reaction is violent, the multi-channel microreactor provided by the utility model has the defects that a large amount of heat is required to be moved in or out at the position close to the inlet and the distribution chamber, and the problem can only be solved by increasing the whole heat exchange volume of the microchannel reaction system.
Disclosure of Invention
The to-be-solved technical problem of the utility model is to provide a micro-reactor, can strengthen mixing and heat transfer function, regulate and control the reaction temperature of the local position in the microchannel reactor effectively. The method is suitable for synthesizing the polyalphaolefin base oil.
In order to achieve the above object, the present invention provides a microchannel reactor, which comprises at least one pre-mixing chamber 3, at least one mixing reaction chamber 6 and a reaction unit connected in series, wherein the pre-mixing chamber is provided with a first inlet of the pre-mixing chamber and a second inlet of the pre-mixing chamber, the mixing reaction chamber is further provided with an inlet of the mixing chamber, the reaction unit comprises a distribution chamber 8, a plurality of parallel reaction channels 9 and a collection chamber 10 which are communicated in sequence, an outlet of the last mixing reaction chamber is communicated with the distribution chamber, and the collection chamber 10 is provided with an outlet 11.
The utility model provides a microchannel reactor's beneficial effect does:
the utility model provides a microchannel reactor is applicable to the reaction that multiple gas-liquid looks raw materials participated in, divide into two stages with the mixing process of reaction raw materials, realizes the mixture and the preparation of first kind of raw materials and catalyst in the first stage, and the second stage realizes the mixture of second kind of raw materials and catalyst. Through two-stage mixing, the one-time reaction of various materials is realized in the same microreactor, and the mixing effect of each stage is enhanced.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a schematic flow diagram of a first embodiment of a microchannel reactor according to the present invention;
fig. 2 is a schematic flow chart of a second embodiment of the microchannel reactor provided by the present invention.
Description of reference numerals:
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are given by way of illustration and explanation only, not limitation.
The utility model provides a microchannel reactor, including at least one of the series connection of order pre-mix room 3, at least one mix reaction chamber 6 and reaction unit, pre-mix the room and be equipped with the first entry of pre-mix room, pre-mix the room second entry, the mixed reaction chamber still be equipped with the mixing chamber entry, the reaction unit by the distribution room 8 of order intercommunication, many parallelly connected reaction channel 9 and collect room 10 and constitute, the mixed reaction chamber export at end with the distribution room communicate with each other, collection room 10 be equipped with export 11.
Optionally, the utility model provides a microchannel reactor includes the room 3, the mixing reaction chamber 6 and the reaction unit of premixing that the order is established ties, and the first entry of premixing room, premixing room second entry communicate with the room 3 of premixing, and the room export of premixing, mixing reaction chamber entry communicate with the mixing reaction chamber.
Preferably, the microchannel reactor provided by the utility model further comprises a heat exchange layer surrounding the outside of the premixing chamber, the mixing reaction chamber and the reaction unit, wherein the heat exchange layer is respectively provided with a plurality of heat exchange medium inlets and a plurality of heat exchange medium outlets.
Preferably, a first heat exchange medium inlet, a second heat exchange medium inlet, a third heat exchange medium inlet and a fourth heat exchange medium inlet are respectively arranged on the heat exchange layer at axial positions before the second inlet of the premixing chamber, before the inlet of the mixing reaction chamber, before the distribution chamber and after the distribution chamber.
The utility model provides a microchannel reactor's a preferred embodiment, pre-mixing chamber 3 in be equipped with first intensive mixing component 4, be equipped with the second in the mixing reaction room 6 and strengthen mixing component 7, first, second are strengthened mixing component and are porous structure.
The first and second intensive mixing elements may be in the form of mesh, slit, or foam or sintered metal. Preferably a foamed metal or a sintered metal.
Preferably, in the mixing chamber, the ratio of the volume of the second intensive mixing element to the volume of the mixing chamber is 1:1 to 5, more preferably 1:1 to 2.
In the microchannel reactor provided by the present invention, preferably, the heat exchange layer is internally provided with the mutually staggered heat exchange partition plates 18. The purpose is to strengthen the heat exchange effect of the strong heat release area.
The heat exchange partition plates in the heat exchange layer can be uniformly arranged, and can also be densely arranged in the middle. Preferably, the heat exchange layer is divided into four parts by the first heat exchange medium inlet, the second heat exchange medium inlet, the third heat exchange medium inlet and the fourth heat exchange medium inlet, and the installation density ratio of the heat exchange partition plates in the four parts is 1:1 to 5:1 to 10:1 to 5:1 to 4.
The heat exchange layer is within the confines of the microchannel reactor shell 12, excluding the above-mentioned internals, and the remainder are channels and regions for heat exchange fluid.
The invention provides an application method of a microchannel reactor, wherein a first raw material enters a premixing chamber through a first inlet of the premixing chamber, a second raw material enters the premixing chamber through a second inlet of the premixing chamber and is uniformly mixed in the premixing chamber, a mixed material flow enters a mixing reaction chamber and is mixed and reacted with a third raw material, the reacted material flow enters a reaction unit and enters a plurality of reaction channels connected in parallel after being distributed in a distribution chamber for reaction, and the reacted material flow enters a collection chamber and is discharged out of the microchannel reactor through an outlet. The utility model provides a microchannel reactor is applicable to the strong exothermic or endothermic reaction, and heat transfer medium lets in at the heat transfer medium entry, and the temperature of room, mixed reaction chamber and reaction unit is in the target range in advance in the control to obtain high quality product.
The utility model provides a microchannel reactor is applicable to the homogeneous reaction that has the stranded material to and have the heterogeneous reaction of multiple gas-liquid, gas-liquid mixture, be applicable to that reaction rate is fast, local heat release or the system that the heat absorption capacity is very big. Is especially suitable for the synthesis process of the polyalphaolefin base oil.
The synthesis method of the poly-alpha olefin base oil comprises the following steps:
(1) Introducing a catalytic promoter and a gas phase catalyst into a first inlet of a premixing chamber and a second inlet of the premixing chamber of the microchannel reactor, and completely mixing in the premixing chamber to form a catalyst mixed fluid;
(2) Introducing a raw material containing a polymerized monomer into an inlet of a mixing reaction chamber of the microchannel reactor, mixing the raw material containing the polymerized monomer and a catalyst mixing fluid in the mixing reaction chamber, introducing the mixture into a distributor of a reaction unit to be dispersed in each reaction channel, further carrying out polymerization reaction, introducing the reacted material flow into a collection chamber, and obtaining a product through an outlet.
In the synthesis method of the polyalphaolefin base oil, the reaction temperature is 0-50 ℃, the reaction pressure is 1.5-4.0MPa, and the reaction time is 0.1-10min.
The raw material containing the polymerized monomer comprises C8-C12 alpha olefin.
The catalytic promoter is alcohol or alkyl ester or the mixture of the two substances. The weight ratio of the amount of the catalytic assistant to the olefin as the raw material is 0.01-1.0%; BF (BF) generator 3 The molar ratio of the dosage to the catalytic promoter is 0.5 to 3.
Compared with the prior art, the utility model provides a microchannel reactor's beneficial effect does:
the utility model provides a microchannel reactor includes multistage mixing chamber, can accomplish the effective mixture of multiple material in same reactor, reduces in the result distribution that brings because the mixing problem.
The heat exchange medium can be added into the microchannel reactor through a plurality of stages of inlets, and the heat exchange grid plates are arranged according to the heat release or heat absorption characteristics of the system, so that the reaction temperature of a strong heat exchange system, especially a multichannel strong heat exchange system, can be effectively controlled, and the product selectivity is improved.
The microchannel reactor has compact structure and small occupied area, can save a large amount of early investment and reduce the operation cost. The liquid storage capacity of the micro-channel reactor system is low, and the safety risk is reduced.
The following further describes a specific embodiment of the microchannel reactor provided by the present invention with reference to the attached drawings.
Fig. 1 is a schematic structural diagram of a first embodiment of a microchannel reactor provided by the present invention, as shown in fig. 1, the microchannel reactor includes: the device comprises a preparation mixing chamber 3, a mixing reaction chamber 6 and a reaction unit which are connected in series, wherein the reaction unit consists of a distribution chamber 8, a plurality of reaction channels 9 which are connected in parallel and a collection chamber 10, and the collection chamber is provided with an outlet 11. The micro-reactor shell 12 is internally provided with a heat exchange layer, the heat exchange layer is provided with a first heat exchange medium inlet 13, a second heat exchange medium inlet 14, a third heat exchange medium inlet 15 and a fourth heat exchange medium inlet 16 along the fluid flowing direction, and a plurality of heat exchange partition plates 18 are arranged in the heat exchange layer in a staggered mode so as to enhance the heat exchange efficiency of heat exchange.
Taking the synthesis method of the polyalphaolefin base oil as an example, the fluid containing the catalytic assistant and the gas-phase catalyst are respectively introduced into the premixing chamber 3 of the microchannel reactor to be mixed, so as to prepare the mixed catalyst with higher catalytic activity. Better mixing with the alpha olefin feedstock entering via mixing chamber inlet 5 is obtained in mixing chamber 6. Through the action of the two-stage intensified mixing components, the three substances finally entering the distribution chamber 8 obtain excellent mixing quality, and meanwhile, the gas-phase catalyst is broken into bubbles with the diameter of less than 1 mm.
The first heat exchange medium inlet 13 introduces a heat exchange medium for basic heat exchange of the whole microreactor system. In the mixing chamber 6, the raw material is initially contacted with the catalyst, a violent chemical reaction occurs, a large amount of heat is generated, and a second heat exchange medium inlet 14 introduces a second strand of heat exchange medium for removing the heat generated in the stage. The reaction mixture enters the distribution chamber 8 and reacts further, but because the distribution chamber has a larger radius than the mixing chamber 6, where the liquid hold-up is relatively large and the heat of reaction generation is correspondingly large, where the third heat exchange medium is introduced through the third heat exchange medium inlet 15, where the large amount of heat generated is removed in a targeted manner. To further maintain the temperature in the reactor, another heat exchange fluid can be introduced at the fourth heat exchange medium inlet 16 after the distribution chamber.
The reaction is carried out by two-stage mixing, so that better mixed catalyst property and target product selectivity can be obtained. The multi-stage heat exchange medium inlet can solve the problem of strong heat release or strong heat absorption in the process of mixing and reacting for multiple times according to local conditions, and better maintains the reaction temperature.
Fig. 2 is a schematic flow diagram of a second embodiment of the microchannel reactor provided by the present invention, which is different from fig. 1 in that the product enters the outlet 11 through the collection chamber and enters the product separator 19, the separated catalyst is recycled through the catalyst outlet 20, and the reaction product enters the subsequent system through the product outlet 21.
The structure and technical effects of the microchannel reactor provided by the present invention will be described by way of example.
The product distribution and conversion analyses in the following examples were determined by off-line chromatographic methods using an agilent GC6890-SCD instrument.
The process that takes place in the following examples is a polyalphaolefin synthesis process using 1-decene as the polymerization raw material, 1-butanol as the catalyst promoter, and BF as the catalyst 3 。
The following conversion was calculated: the product is cooled to room temperature and transferred to a separating funnel, and after adding NaOH solution and a small amount of distilled water, the mixture is shaken up and stands still. After the water layer is separated out, the pH value of the water layer is detected by using a pH test paper. Repeating the operation until the pH value of the water layer is 7, and standing for a period of time. After all the water is separated out, separating and directly carrying out liquid chromatography analysis. Feed conversion = 1-decene concentration in product/1-decene concentration in feed.
The following selectivity was calculated: the product is cooled to room temperature and transferred to a separating funnel, and after adding NaOH solution and a small amount of distilled water, the mixture is shaken up and stands still. After the water layer is separated out, the pH value of the water layer is detected by using a pH test paper. Repeating the operation until the pH value of the water layer is 7, and standing for a period of time. Separating after water is completely separated out, directly carrying out liquid chromatography analysis, and respectively measuring the concentrations of the monomer, the dimer, the trimer and the tetramer in the product. Selectivity for each product (N-mer) = concentration of N-mer in product/feed conversion.
Comparative example 1
The test method comprises the following steps: purging the reaction kettle with nitrogen, adding 20 mL of 1-decene into a stainless steel stirred tank reactor, dropwise adding 0.2mL of n-butanol, and introducing BF 3 And gas bubbling on the liquid surface. The reaction was carried out at 30 ℃ for 4 hours under a reaction pressure of 0.4MPa, and the reaction was terminated.
The conversion and product distribution of the reaction are shown in table 1.
Example 1
This example uses the microchannel reactor system shown in FIG. 1 for the synthesis of polyalphaolefin base oils.
The process flow in this example is as described in the foregoing preferred embodiments of the present invention, and other relevant matters are as follows:
in the microchannel reactor, the reactor was equipped with eight microchannels having a length of 2.0m, the preliminary mixing chamber 3 was 200mm long, the reaction mixing chamber 6 was 200mm long, and the distribution chamber 8 and the collection chamber 10 were cylindrical structures having a bottom surface diameter of 110mm and a height of 15 mm. The liquid-phase auxiliary agent inlet passage 2 and the raw material inlet passage 5 are respectively located at the edge positions of the preparatory mixing chamber 3 and the reaction mixing chamber 6.
The micro-reactor system is provided with a first heat exchange medium channel, a second heat exchange medium inlet channel, a third heat exchange medium inlet channel and a fourth heat exchange medium inlet channel. The first heat exchange medium inlet channel is located at the position of the gas-phase catalyst inlet channel 1 close to the downstream, the second heat exchange medium inlet channel is located at the position 20mm in front of the raw material inlet channel 5, the third heat exchange medium inlet channel is located at the position 20mm in front of the distribution chamber 8, and the fourth heat exchange medium inlet channel is located at the position 30mm behind the raw material distribution chamber 8. The flow ratio of each heat exchange medium =1:2:5:2.
BF3, 1-decene and 1-butanol enter the microchannel reactor from a gas phase catalyst inlet channel 1, a liquid phase auxiliary agent inlet channel 2 and a raw material inlet channel 5 in the figure 1 respectively to carry out polymerization reaction, and the obtained reaction product is led out from an outlet 11.
The reaction temperature in the test method according to this example was substantially the same as that in comparative example 1, and the reaction pressure was 2.5MPa. In addition, in this example, the feed rate of 1-decene was 10mL/min, the feed rate of n-butanol was 0.1mL/min, and BF was measured 3 The feeding speed of (2) is 40mL/min, and after reactants are fed for 10min, stable product discharge is obtained, and the product properties are shown in Table 1.
TABLE 1
| Example 1 | Comparative example 1 | |
| Conversion (%) | 90.51 | 90.35 |
| Dimer yield (%) | 11.72 | 13.97 |
| Trimer yield (%) | 34.76 | 32.77 |
| Tetramer yield (%) | 26.56 | 24.69 |
| Pentameric yield (%) | 13.59 | 15.03 |
| >Pentameric yield (%) | 3.85 | 3.84 |
The results in table 1 show that, compared to conventional batch tank reactors, higher feedstock conversion can be achieved with the microchannel reactor of the present invention and that the selectivity of trimers and tetramers in the product is significantly superior to batch tank technology. In addition, the reaction time can be reduced from 4h to 10min, enabling continuous flow production of polyalphaolefins. Compare with the microchannel reactor who does not possess the preliminary mixing chamber to and the multichannel microreactor that does not possess multistage heat transfer medium entry, the selectivity of trimerization complete and tetramer in the product obtains obviously improving, explains the utility model discloses a microchannel reactor structure has obtained obvious optimization, more is fit for poly alpha olefin reaction process.
Claims (10)
1. The microchannel reactor is characterized by comprising at least one premixing chamber (3), at least one mixing reaction chamber (6) and a reaction unit which are sequentially connected in series, wherein the premixing chamber is provided with a first inlet of the premixing chamber and a second inlet of the premixing chamber, the mixing reaction chamber is further provided with a mixing chamber inlet, the reaction unit consists of a distribution chamber (8), a plurality of reaction channels (9) and a collection chamber (10) which are sequentially communicated, an outlet of the mixing reaction chamber is communicated with the distribution chamber, and the collection chamber (10) is provided with an outlet (11).
2. The microchannel reactor according to claim 1, comprising a premixing chamber (3), a mixing reaction chamber (6) and a reaction unit connected in series in this order, wherein a first inlet of the premixing chamber and a second inlet of the premixing chamber are communicated with the premixing chamber (3), and an outlet of the premixing chamber and an inlet of the mixing reaction chamber are communicated with the mixing reaction chamber.
3. The microchannel reactor according to claim 1 or 2, further comprising a heat exchange layer surrounding the outside of the premixing chamber, the mixing reaction chamber and the reaction unit, wherein the heat exchange layer is provided with a plurality of heat exchange medium inlets, respectively.
4. The microchannel reactor according to any of claims 1 or 2, wherein the premixing chamber (3) is provided with a first intensive mixing element (4) and the mixing reaction chamber (6) is provided with a second intensive mixing element (7), said first and second intensive mixing elements being of porous structure.
5. The microchannel reactor of claim 4 wherein the first and second intensive mixing members are either foamed metal or sintered metal.
6. The microchannel reactor of claim 4 wherein the mixing chamber has a ratio of the volume of the second intensive mixing element to the volume of the mixing chamber of 1:1 to 5.
7. The microchannel reactor of claim 6, wherein the ratio of the volume of the second intensive mixing element to the volume of the mixing chamber is 1:1 to 2.
8. The microchannel reactor of claim 3 wherein the heat exchange layers have interleaved heat exchange baffles (18).
9. The microchannel reactor of claim 8, wherein the heat exchange layer is divided into four sections by the first heat exchange medium inlet, the second heat exchange medium inlet, the third heat exchange medium inlet, and the fourth heat exchange medium inlet, and a ratio of installation densities of the heat exchange partitions in the four sections is 1:1 to 5:1 to 10:1 to 5:1 to 4.
10. The microchannel reactor according to claim 1 or 2, wherein the flow cross-sectional area of the single reaction channel (9) is 0.001mm 2 -6mm 2 The ratio of the inner diameter to the length of the reaction channel (9) is 1:100-30000.
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