CN105817187A - Microchannel reaction apparatus and system suitable for extreme exothermic reactions - Google Patents
Microchannel reaction apparatus and system suitable for extreme exothermic reactions Download PDFInfo
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- CN105817187A CN105817187A CN201610005993.0A CN201610005993A CN105817187A CN 105817187 A CN105817187 A CN 105817187A CN 201610005993 A CN201610005993 A CN 201610005993A CN 105817187 A CN105817187 A CN 105817187A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 137
- 239000012530 fluid Substances 0.000 claims description 82
- 230000003068 static effect Effects 0.000 claims description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 229910000856 hastalloy Inorganic materials 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000003754 machining Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000006396 nitration reaction Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GOYDNIKZWGIXJT-UHFFFAOYSA-N 1,2-difluorobenzene Chemical compound FC1=CC=CC=C1F GOYDNIKZWGIXJT-UHFFFAOYSA-N 0.000 description 2
- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- ZWWCURLKEXEFQT-UHFFFAOYSA-N dinitrogen pentoxide Inorganic materials [O-][N+](=O)O[N+]([O-])=O ZWWCURLKEXEFQT-UHFFFAOYSA-N 0.000 description 2
- YVPJCJLMRRTDMQ-UHFFFAOYSA-N ethyl diazoacetate Chemical compound CCOC(=O)C=[N+]=[N-] YVPJCJLMRRTDMQ-UHFFFAOYSA-N 0.000 description 2
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MPXDAIBTYWGBSL-UHFFFAOYSA-N 2,4-difluoro-1-methylbenzene Chemical compound CC1=CC=C(F)C=C1F MPXDAIBTYWGBSL-UHFFFAOYSA-N 0.000 description 1
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical compound FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010129 solution processing Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
- B01J2219/00792—One or more tube-shaped elements
- B01J2219/00797—Concentric tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00889—Mixing
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a microchannel reaction device and a microchannel reaction system suitable for extreme exothermic reaction, wherein the microchannel reaction device suitable for extreme exothermic reaction comprises a first pipe body and a second pipe body, a first heat exchange cavity is formed inside the first pipe body, a plurality of microchannel reaction grooves are arranged on the outer surface of the first pipe body, the outer pipe surface of the first pipe body is matched with the inner pipe surface of the second pipe body, and the inner pipe surface of the second pipe body is just sleeved on the outer pipe surface of the first pipe body, so that the microchannel reaction grooves are closed to form a plurality of reaction microchannels. Simple structure, convenient manufacture, low cost and high yield.
Description
Technical field
The present invention relates to microchannel reaction unit and the system of a kind of applicable very exothermic reaction, and can be according to the treating capacity of reaction system, industrialization production requirements is met, it is possible to multiple series connection realize needing the most long reaction process by the change of unary increase and structure.Belong to the technical field of micro passage reaction.
Background technology
Process the industrial conventional aluminum fin heat exchanger of chemical system of exothermic reaction at present, the device such as stainless steel plate type heat exchanger or fin-tube type heat exchanger, all there is certain limitation, as the reaction system of Fast exothermic in the short time can not be processed, or device materials is limited, can not use some corrosive liquids, therefore a lot of occasions are restricted.Along with the rise of micro passage reaction, the most in the ascendant to its application in laboratory both at home and abroad.Substantially using the passage of metal rustless steel etching, use sandwich structure to be made like the scaled down version structure of plate type heat exchanger, treating capacity is little, and structure is complicated, and difficulty of processing is big, and installation cost is high, is unfavorable for industrial applications.
It is contemplated that by traditional polish means, it is possible to use advanced moulding process, produce applicable laboratory and microchannel reaction unit useful industrially, be suitable for the condition of some very exothermic reaction.Micro-channel heat exchanger is because of its great reference area, and superpower heat exchange property is the most more and more paid attention to.But in actual industrial uses, be not widely used.The microchannel reaction apparatus structure of the present invention is novel simple, easily prepares, and cost of manufacture is cheap, and can be widely used in the system of industrialization very exothermic.This device has bigger application prospect in chemical field.In addition this equipment belongs to miniature chemical machinery category, can be widely applied to microfluidic field so that whole equipment miniaturization, miniaturization, it is possible in laboratory field, is engaged in commercial scale and amplifies, and without traditional enlarge-effect.
Summary of the invention
Goal of the invention: it is an object of the invention to provide a kind of novel simple, easily prepare, cost of manufacture is cheap, and can be widely used in microchannel reaction unit and the system of the system of industrialization very exothermic.
During present invention is mainly applied to fluid reaction, its reaction is along with quick heat release.Reaction can be had a negative impact by these heats, and therefore heat have to remove in system as early as possible, not so easily causes the incomplete of reaction, and serious will result in danger.Overcome some drawbacks of prior device, select carborundum, rustless steel, titanium, Hastelloy, carbon fiber board or other resistant materials to prepare.Can be applicable to some reaction systems and equipment and materials is had the occasion of certain particular/special requirement.
Technical scheme: the microchannel reaction unit of applicable very exothermic of the present invention reaction, including the first body, the second body, described first body be internally formed the first heat exchanging chamber, the outer surface of described first body is provided with some microchannels reactive tank, the outer tube surface of the first body and the second body inner tube surface cooperate, and second the inner tube surface of body be just enclosed within the outer tube surface of the first body so that reactive tank Guan Bi in described some microchannels forms some microchannel.Simple in construction, it is convenient to manufacture, low cost, and yield rate is high.
Further, also including the 3rd body, the diameter of described 3rd body is more than the diameter of described second body, and described 3rd body is enclosed within outside the second body, forms the second heat exchanging chamber between the 3rd body and the second body.
Further, one end of described first body is provided with the first heat exchanging fluid entrance being communicated to the first heat exchanging chamber, and the other end of described first body is provided with the first heat exchanging fluid outlet being communicated to the first heat exchanging chamber；Being provided with reacting fluid entrance and reacting fluid outlet on described second body, described reacting fluid entrance is connected to one end of described some microchannel, and the outlet of described reacting fluid is connected to the other end of described some microchannel.
Further, described 3rd body is provided with the second heat exchanging fluid entrance being connected to the second heat exchanging chamber and the second heat exchanging fluid outlet being connected to the second heat exchanging chamber.
Further, also include that static mixer, described static mixer are arranged in described first heat exchanging chamber.
Further, the width of described microchannel is 0.05mm～5mm, and the degree of depth is 0.1mm～5mm, and microchannel length is equal with the 3rd tube length.
Further, the outer tube surface of described first body and the second body the distance of inner tube surface be 0.08-0.12 machining fitted position.
Further, described second body is carborundum, rustless steel, titanium, Hastelloy or carbon fiber board tubulation body.
Further, described static mixer is SK, SV, SX, SL or SH type static mixer.
Further, including some microchannel reaction units being exported the described applicable very exothermic reaction being sequentially connected in series by described reacting fluid entrance and described reacting fluid.
Compared with prior art, it provides the benefit that the present invention: common micro passage reaction usually difficulty of processing is relatively big, and the easily damaged yield rate of the course of processing is low causes production cost high.And need the complicated processing steps such as bonding.And the microchannel of the present invention is reacted it and is needed only to be processed to form some microchannels reaction geosynclinal concave groove at the first tube wall of the most breakable tubulose, and this microchannel reactive tank is at the outer wall of body, it is more easy to processing, is then not required to additional bonds, micro passage reaction can be formed by socket.Using coaxial three-decker, this invention finally makes some projects need not put into bigger fund, it is possible to fully obtains the use characteristic of this micromodule equipment, is substantially reduced Project in Operation and maintenance cost.
The present invention can solve the problem that the problem that quickly removes of a large amount of reaction heat strongly exothermic switching phase released, thus realizes the accurate control to strong exothermal reaction phase temperature, eliminates potential safety hazard, improves reaction selectivity.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the microchannel reaction unit of applicable very exothermic of the present invention reaction；
Fig. 2 is the schematic cross-section of the microchannel reaction unit of applicable very exothermic of the present invention reaction；
Fig. 3 is the microchannel reaction system schematic that the present invention is suitable for very exothermic reaction.
Detailed description of the invention
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1
The microchannel reaction unit of the applicable very exothermic reaction of the present embodiment, this device is coaxial three-decker, is followed successively by the first body the 1, second body 4 and the 3rd body 11 from the inside to the outside.First body 1 is a straight tube, and its one end is the first heat exchanging fluid entrance 2, and the other end is the first heat exchanging fluid outlet 10.Heat exchanging fluid enters the first heat exchanging chamber within the first body 1 by heat exchanging fluid entrance 2, is taken away by heat from heat exchanging fluid outlet 10 outflow.First body 10 outer wall is machined with some microchannels reactive tank, and the second body 4 is enclosed within the outer wall of the first body 10 just, so makes the second inboard wall of tube body be closed by microchannel reactive tank, forms some microchannel 5.Microchannel 5 one terminates reacting fluid entrance 7, another termination reacting fluid outlet 9, and reacting fluid is entered after microchannel 5 is reacted through by reacting fluid outlet 9 derivation by reacting fluid entrance 7.
3rd body 11 is enclosed within second body 4 one the second heat exchanging chamber of outer formation again, and equally, the heat exchanging fluid in the second heat exchanging chamber is flowed into by the second heat exchanging fluid entrance 6, by the second heat exchanging fluid outlet 8 outflow, takes away heat.
Static mixer 4 it is provided with in first body.Cavity is entered when reaction mass carries amount of heat from reacting fluid entrance 7 entrance, now a large amount of low temperature cold fluid the first heat exchanging fluid entrances 2 and the second heat exchanging fluid entrance 6 enter device, heat exchange is carried out by the microchannel 5 of the first body 1 surrounding, cold flow body is through the flow-disturbing of static mixer 3, can be quickly by the fluid boundary damage layer in the first body 1 inner pipe wall, tube fluid is made to carry out the exchange of heat and material at axial direction, thus significantly more efficient heat exchange.
Embodiment 2
Series connection two or more is suitable for the microchannel reaction unit of very exothermic reaction, reaction mass enters from reacting fluid entrance 7 and carries amount of heat entrance cavity, low temperature cold fluid enters device from the first heat exchanging fluid entrance 2 and second heat exchanging fluid entrance 6 mouth of pipe, heat exchange is carried out by the microchannel 5 of the first body 1 tube wall surrounding, the reacting fluid entrance 7 of the microchannel reaction unit that reacting fluid outlet 9 is reacted with second applicable very exothermic is connected, first heat exchanging fluid entrance 2 of the microchannel reaction unit that the first heat exchanging fluid outlet 10 of the microchannel reaction unit of first applicable very exothermic reaction is reacted with second applicable very exothermic is connected.For ensureing the consistent of reaction temperature, the first heat exchanging fluid entrance 2 and the second heat exchanging fluid entrance 6 use the cold flow source of same temperature.
Embodiment 3
Use anhydrous nitric acid (> 98%) and concentrated sulphuric acid (> 95%) prepare nitric acid and sulfuric acid molar ratio be 0.3, water concentration be the nitration mixture of 5%.Under normal temperature condition, 50kg/h nitration mixture and 34kg/h phenol are inputted micro-mixer mixing continuously by pump, and within the extremely short time of staying, mixing is fully, then enter, from reacting fluid entrance 7, the micro-heat exchanger arranged for the strong heat exchange stage of reaction and carry out strong heat exchange reaction.This device quickly removes the amount of heat produced in the strong exothermal reaction stage, and in course of reaction, temperature can control at 25 DEG C.React in pumping into microreactor.The mol ratio controlling nitric acid and phenol is 1.8, and the amount of heat that reaction produces is cooled down by cold flow body, and product flows continually out reactor, static layering, separates acid solution, and organic facies carries out washing, alkali cleaning and be washed to neutrality.The temperature of this microchannel reaction unit controls to substantially increase selectivity and the productivity of nitration reaction, and productivity is by 60% raising of popular response to 85%, and the by-products such as selectivity improves to 95%, polymer are less than 3%.
Embodiment 4
The microchannel reaction unit of the applicable very exothermic reaction of two embodiments 3 of series connection, reaction mass enters from reacting fluid entrance 7, low temperature cold fluid enters device from the first heat exchanging fluid entrance 2 and second heat exchanging fluid entrance 6 mouth of pipe, heat exchange is carried out by the microchannel 5 of the first body 1 surrounding, at the reacting fluid of the microchannel reaction unit of first applicable very exothermic reaction, the reacting fluid entrance 7 of the microchannel reaction unit that mouth 9 reacts with second applicable very exothermic is connected, first heat exchanging fluid entrance 2 of the microchannel reaction unit that the first heat exchanging fluid outlet 10 of the microchannel reaction unit of first applicable very exothermic reaction is reacted with second applicable very exothermic is connected.For ensureing the consistent of reaction temperature, the first heat exchanging fluid entrance 2 and the second heat exchanging fluid entrance 6 use the cold flow source of same temperature, and yield promotes 2 times.
Embodiment 5
Micro-reaction device is cooled to 10 DEG C.30.5kg/hN-tertbutyloxycarbonyl-4-piperidones and the dichloromethane/t-butyl methyl ether solution of 21.4L/h ethyl diazoacetate and the t-butyl methyl ether solution input micro-mixer mixing dissolved with 4.3L/h boron triflouride etherate will be dissolved, within the extremely short time of staying, mixing is fully, then enters, from reacting fluid entrance 7, the micro-heat exchanger arranged for the strong heat exchange stage of reaction and carries out strong heat exchange reaction.This device quickly removes the amount of heat produced in the strong exothermal reaction stage, and in course of reaction, temperature can control at 10 DEG C.N-tertbutyloxycarbonyl-4-piperidones and ethyl diazoacetate mol ratio are 0.7.Product is cancellation in aqueous tartaric acid solution, and post processing productivity reaches 92%.
Embodiment 6
The microchannel reaction unit of the applicable very exothermic reaction of two embodiments 5 of series connection, reaction mass enters from reacting fluid entrance 7, low temperature cold fluid enters device from the first heat exchanging fluid entrance 2 and second heat exchanging fluid entrance 6 mouth of pipe, heat exchange is carried out by the microchannel 5 of the first body 1 surrounding, at the reacting fluid of the microchannel reaction unit of first applicable very exothermic reaction, the reacting fluid entrance 7 of the microchannel reaction unit that mouth 9 reacts with second applicable very exothermic is connected, first heat exchanging fluid entrance 2 of the microchannel reaction unit that the first heat exchanging fluid outlet 10 of the microchannel reaction unit of first applicable very exothermic reaction is reacted with second applicable very exothermic is connected.For ensureing the consistent of reaction temperature, the first heat exchanging fluid entrance 2 and the second heat exchanging fluid entrance 6 use the cold flow source of same temperature, and yield promotes 2 times.
Embodiment 7
Use anhydrous nitric acid (> 98%) and concentrated sulphuric acid (> 95%) prepare nitric acid and sulfuric acid molar ratio be 0.3, water concentration be the nitration mixture of 3%.Under normal temperature condition, 30kg/h nitration mixture and 17kg/h toluene are continuously pumped into micro-mixer mixing by pump, and within the extremely short time of staying, mixing is fully, then enter, from 7, the micro-heat exchanger arranged for the strong heat exchange stage of reaction and carry out strong heat exchange reaction.This device quickly removes the amount of heat produced in the strong exothermal reaction stage, and in course of reaction, temperature can control at 25 DEG C.The mol ratio controlling nitric acid and phenol is 2.5, and the amount of heat that reaction produces is cooled down by cold flow body, and product flows continually out reactor, static layering, separates acid solution, and organic facies carries out washing, alkali cleaning and be washed to neutrality.The temperature of this microchannel reaction unit controls to substantially increase selectivity and the productivity of dinitrotoluene (DNT), and productivity is by 80% raising of popular response to 97%, and selectivity improves to 99%.
Embodiment 8
The microchannel reaction unit of the applicable very exothermic reaction of three embodiments 7 of series connection, reaction mass enters from reacting fluid entrance 7, low temperature cold fluid enters device from the first heat exchanging fluid entrance 2 and second heat exchanging fluid entrance 6 mouth of pipe, heat exchange is carried out by the microchannel 5 of the first body 1 surrounding, at the reacting fluid of the microchannel reaction unit of first applicable very exothermic reaction, the reacting fluid entrance 7 of the microchannel reaction unit that mouth 9 reacts with second applicable very exothermic is connected, first heat exchanging fluid entrance 2 of the microchannel reaction unit that the first heat exchanging fluid outlet 10 of the microchannel reaction unit of first applicable very exothermic reaction is reacted with second applicable very exothermic is connected.For ensureing the consistent of reaction temperature, the first heat exchanging fluid entrance 2 and the second heat exchanging fluid entrance 6 use the cold flow source of same temperature, and yield promotes 2 times.
Embodiment 9
O-difluoro-benzene/the tetrahydrochysene of the 15wt% of 12.5kg/h is barked mixed solution of muttering, and the hexyl of the 33wt% of 5.0kg/h bury/mixed solution of hexane inputs reaction unit the most continuously,-40 DEG C it are cooled to respectively through precooler, the temperature that the temperature with o-difluoro-benzene drops to react required respectively will be buried by hexyl, then input micro-mixer mixing, within the extremely short time of staying, mixing is fully, then enters, from 7, the micro-heat exchanger arranged for the strong heat exchange stage of reaction and carries out strong heat exchange reaction.This device quickly removes the amount of heat produced in the strong exothermal reaction stage, and in course of reaction, temperature can control at about-40 DEG C.Bark with the dimethyl sulfate/tetrahydrochysene of the 40wt% being pre-chilled to-40 DEG C that flow is 6.7kg/hr mixed solution of muttering of the product produced after this step reaction mixes in another micro-mixer, entering back in two heat exchangers that another group is linked in sequence and react, reaction temperature controls at-40 DEG C.Reaction exports end product neighbour's difluoro toluene after terminating.Reaction selectivity is 94%.
Above-described embodiment shows to apply reaction unit of the present invention and method, can solve the problem that the problem that quickly removes of a large amount of reaction heat strongly exothermic switching phase released, thus realize the accurate control to strong exothermal reaction phase temperature, eliminate potential safety hazard, improve reaction selectivity.
Although as it has been described above, represented and described the present invention with reference to specific preferred embodiment, but it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention premise defined without departing from claims, can various changes can be made in the form and details to it.
Claims (10)
1. the microchannel reaction unit of an applicable very exothermic reaction, it is characterized in that, including the first body (1), second body (4), described first body (1) be internally formed the first heat exchanging chamber, the outer surface of described first body (1) is provided with some microchannels reactive tank, the outer tube surface of the first body (1) and the second body (4) inner tube surface cooperate, and second the inner tube surface of body (4) be just enclosed within the outer tube surface of the first body (1), described some microchannels reactive tank Guan Bi is made to form some microchannel (5).
The microchannel reaction unit of applicable very exothermic the most according to claim 1 reaction, it is characterized in that, also include the 3rd body (11), the diameter of described 3rd body (11) is more than the diameter of described second body (4), described 3rd body (11) is enclosed within the second body (4) outward, forms the second heat exchanging chamber between the 3rd body (11) and the second body (4).
The microchannel reaction unit of applicable very exothermic the most according to claim 1 reaction, it is characterized in that, one end of described first body (1) is provided with the first heat exchanging fluid entrance (2) being communicated to the first heat exchanging chamber, and the other end of described first body (1) is provided with the first heat exchanging fluid outlet (10) being communicated to the first heat exchanging chamber；Reacting fluid entrance (7) and reacting fluid outlet (9) it is provided with on described second body (4), described reacting fluid entrance (7) is connected to one end of described some microchannel (5), and the outlet of described reacting fluid is connected to the other end of described some microchannel (5).
The microchannel reaction unit of applicable very exothermic the most according to claim 2 reaction, it is characterized in that, described 3rd body (11) is provided with the second heat exchanging fluid entrance (6) being connected to the second heat exchanging chamber and the second heat exchanging fluid outlet (8) being connected to the second heat exchanging chamber.
The microchannel reaction unit of applicable very exothermic the most according to claim 1 reaction, it is characterised in that also include that static mixer (3), described static mixer (3) are arranged in described first heat exchanging chamber.
6. according to the microchannel reaction unit of the arbitrary described applicable very exothermic reaction of Claims 1 to 5, it is characterized in that, the width of described microchannel (5) is 0.05mm～5mm, the degree of depth is 0.1mm～5mm, and microchannel (5) length is equal with the 3rd body (11) length.
7. according to the microchannel reaction unit of the arbitrary described applicable very exothermic reaction of Claims 1 to 5, it is characterized in that, the outer tube surface of described first body (1) and the second body (4) the distance of inner tube surface be 0.08-0.12 machining fitted position.
8. according to the microchannel reaction unit of the arbitrary described applicable very exothermic reaction of Claims 1 to 5, it is characterised in that described second body (2) is carborundum, rustless steel, titanium, Hastelloy or carbon fiber board tubulation body.
The microchannel reaction unit of applicable very exothermic reaction the most according to claim 5, it is characterised in that described static mixer is SK, SV, SX, SL or SH type static mixer.
10. according to the microchannel response system of the arbitrary described applicable very exothermic reaction of Claims 1 to 5, it is characterized in that, including some microchannel reaction units being exported the described applicable very exothermic reaction that (9) are sequentially connected in series by described reacting fluid entrance (7) and described reacting fluid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610005993.0A CN105817187A (en) | 2016-01-05 | 2016-01-05 | Microchannel reaction apparatus and system suitable for extreme exothermic reactions |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610005993.0A CN105817187A (en) | 2016-01-05 | 2016-01-05 | Microchannel reaction apparatus and system suitable for extreme exothermic reactions |
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| CN105817187A true CN105817187A (en) | 2016-08-03 |
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| CN201610005993.0A Pending CN105817187A (en) | 2016-01-05 | 2016-01-05 | Microchannel reaction apparatus and system suitable for extreme exothermic reactions |
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| CN107413286A (en) * | 2017-02-04 | 2017-12-01 | 青岛大学 | Disposable thermostabilization microresponse device |
| CN108176335A (en) * | 2018-03-07 | 2018-06-19 | 厦门大学 | Tandem microreactor with hole-groove combined microchannel porous metals reaction carriers |
| CN108993343A (en) * | 2018-09-06 | 2018-12-14 | 山东豪迈机械制造有限公司 | A kind of micro passage reaction |
| WO2021035796A1 (en) * | 2019-08-30 | 2021-03-04 | 欧志安 | Pressurized fluid mixing device |
| CN114797702A (en) * | 2021-01-18 | 2022-07-29 | 万华化学集团股份有限公司 | Continuous microchannel reactor for olefin epoxidation reaction and olefin epoxidation reaction method |
| CN108047033B (en) * | 2017-12-20 | 2023-12-01 | 江西科苑生物药业有限公司 | Reaction device and method for preparing mandelic acid compound |
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| CN114797702A (en) * | 2021-01-18 | 2022-07-29 | 万华化学集团股份有限公司 | Continuous microchannel reactor for olefin epoxidation reaction and olefin epoxidation reaction method |
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