CN216935945U - Reaction device for multiphase system - Google Patents
Reaction device for multiphase system Download PDFInfo
- Publication number
- CN216935945U CN216935945U CN202120748028.9U CN202120748028U CN216935945U CN 216935945 U CN216935945 U CN 216935945U CN 202120748028 U CN202120748028 U CN 202120748028U CN 216935945 U CN216935945 U CN 216935945U
- Authority
- CN
- China
- Prior art keywords
- liquid
- reactor
- inlet
- outlet
- separator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 78
- 239000007788 liquid Substances 0.000 claims abstract description 90
- 239000003054 catalyst Substances 0.000 claims abstract description 56
- 239000007787 solid Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000012528 membrane Substances 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- 230000005484 gravity Effects 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 103
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 24
- 238000001914 filtration Methods 0.000 description 18
- 238000000926 separation method Methods 0.000 description 17
- 239000002994 raw material Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 13
- 238000002156 mixing Methods 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 238000011001 backwashing Methods 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 5
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000009295 crossflow filtration Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000012465 retentate Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Landscapes
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The utility model discloses a reaction device for a multiphase reaction system, which consists of an equal-diameter riser reactor (5), a liquid-solid separator (8), a liquid-liquid separator (13) and a tubular mixer (4), wherein the bottom of the riser reactor is provided with a dispersed phase inlet (1) and a catalyst discharge outlet (6), the top of the reactor is communicated with the inlet of the solid-liquid separator through an external circulating pipe (7), a trapped liquid outlet of the solid-liquid separator is communicated with the bottom of the reactor through the tubular mixer, a clear liquid outlet (10) of the solid-liquid separator is communicated with the inlet of the liquid-liquid separator, the liquid-liquid separator is provided with a water phase outlet and an oil phase outlet, and the water phase outlet or the oil phase outlet is communicated with the inlet of the tubular mixer (4). The reaction device for the multiphase system provided by the utility model strengthens liquid-liquid mass transfer, realizes the circular flow of the catalyst in the reactor, and can improve the reaction efficiency and realize the long-period operation of the device.
Description
Technical Field
The utility model relates to chemical process equipment, in particular to a reaction device suitable for a liquid-solid multiphase reaction system.
Background
The solid phase catalytic reaction is an important reaction means, and the related reaction system can cover gas-solid, liquid-solid, gas-liquid-solid and heterogeneous systems containing immiscible liquid-liquid, etc., wherein the liquid-liquid heterogeneous reaction process with the participation of the solid phase catalyst is widely applied to the engineering fields of petrochemical industry, biological reaction, environmental protection, etc., and one of the keys of the liquid-solid heterogeneous reaction is to ensure the high-efficiency mixing of the liquid-liquid two phase and fully contact with the solid phase catalyst, thereby improving the reaction rate.
For liquid-liquid mixing process intensification, physical disruption and chemical dissolution-assisting methods are generally used. The industry generally uses mechanical stirring, design of tortuous flow channels, high-speed liquid impact, etc. to generate fluid turbulence to increase the mixing efficiency of the liquid. The most common reactor is a stirred tank, which utilizes the mechanical stirring action of a stirrer to realize the mixing and reaction of raw materials. However, due to the limitation of the stirred tank device, the mixing time scale is between several minutes and even several hours, and the mixing time scale is usually used for reaction systems with slower reaction rate. For example, CN 202527171a discloses a reaction apparatus for gas-liquid-solid heterogeneous reaction, in which a guide shell is installed inside a reactor, and a stirrer is installed inside the guide shell, and the contact reaction of raw materials is realized by means of stirring. US 4289762 discloses mixing two reactants in fan-shaped jets in a cylindrical mixing chamber. The conventional static mixer adopts a tortuous flow passage to intensively mix the fluid, and the mixing effect is relatively poor. Chemical dissolution-assisting methodThe method is to add cosolvent, such as surfactant, alcohols, ethers, ketones and other solvents, to realize liquid-liquid interphase mixing. For example, CN 101293813A adopts emulsifier RC6H5O(CH2CH2O)nH, forming the four carbon components and water into oil-in-water emulsion for hydration reaction. CN101314596A adopts methanol or a mixture of methanol and water to realize the contact mixing of propylene and hydrogen peroxide, and then synthesizes propylene oxide under the catalysis of a titanium silicalite molecular sieve. The addition of non-raw materials has a great influence on the subsequent separation and may also cause side reactions.
For the use of solid phase catalyst, the catalyst is mostly filled in a fixed bed form at present, and the method is characterized in that the filling of the catalyst is difficult, the components in a reactor are complex, and the method is particularly not suitable for the reaction process with quick catalyst deactivation; in addition, the catalyst particles are relatively large and are not beneficial to contact reaction with a liquid-liquid phase, so that the reaction efficiency is low. While the catalyst and one of the liquid phases are prepared into slurry for reaction as described in CN101314596a, which improves the catalytic efficiency, the disadvantage is that the catalyst and the product need to be separated, and the catalyst particles are too small, which results in a complicated separation process and a short back-washing period of the filtering device.
SUMMERY OF THE UTILITY MODEL
The technical problem to be solved by the utility model is to provide a reaction system suitable for a liquid-solid multi-system based on the prior art so as to solve the problems of mixing between liquid and liquid, the performance problem of a catalyst and the phase separation problem of a product.
A reaction device for a multiphase system comprises a riser reactor 5 with equal diameter, a liquid-solid separator 8, a liquid-liquid separator 13 and a tubular mixer 4, wherein the bottom of the riser reactor is provided with a dispersed phase inlet 1 and a catalyst discharge outlet 6, the top of the reactor is communicated with the inlet of the solid-liquid separator through an external circulation pipe 7, the intercepted liquid outlet of the solid-liquid separator is communicated with the bottom of the reactor through the tubular mixer, the clear liquid outlet 10 of the solid-liquid separator is communicated with the inlet of the liquid-liquid separator, the liquid-liquid separator is provided with a water phase outlet and an oil phase outlet, and the water phase outlet or the oil phase outlet is communicated with the inlet of the tubular mixer 4.
The application method of the reaction device for the multiphase system selects the water phase raw material or the oil phase raw material as the disperse phase, and selects the other phase as the continuous phase. The application method of the utility model is illustrated by taking an oil phase raw material as a dispersed phase as an example, the water phase raw material is introduced from a continuous phase inlet, the oil phase raw material enters a reactor from the bottom through the dispersed phase inlet and a dispersed phase feeder, and a reactant flow flows upwards in a cylindrical reactor with equal diameter and generates multi-phase contact reaction. The reaction material flow at the top of the reactor enters the upper section of the external circulation pipe and enters the liquid-solid separator for solid-liquid separation, the slurry flow containing catalyst particles is discharged out of the liquid-solid separator and enters the tubular mixer through the lower section of the external circulation pipe to be mixed with the water phase raw material from the continuous phase inlet and the circulating material at the water phase outlet of the liquid-liquid separator and then enters the bottom of the reactor; clear liquid separated from the liquid-solid separator enters the liquid-liquid separator through a clear liquid outlet to separate an oil phase from a water phase, the separated oil phase is extracted through an oil phase outlet and further separated to obtain a product, and the separated water phase returns to the tubular mixer through a water phase outlet for recycling.
The reaction device for the multiphase reaction system has the advantages that:
the reaction device for the multiphase reaction system provided by the utility model has a simple structure and is suitable for liquid-solid multiphase reaction. (1) The method has the advantages that other surfactants or cosolvents are not required to be added, one phase reactant is dispersed into a tiny liquid through the dispersed phase feeder, and the materials are mixed through the jet mixer, so that the reaction efficiency is improved. (2) The solid phase catalyst with the particle size between the fixed bed and the slurry bed can be adopted, the influence of the surface diffusion and the internal diffusion of the catalyst on the reaction can be reduced to a certain extent, the liquid-solid separation is easier to realize compared with the slurry catalyst, and the back washing period of the filter assembly is favorably prolonged. (3) The solid-phase catalyst is in a circulating flow state in the reactor, so that the online renewal of the catalyst can be realized, and the catalyst can be used for a reaction system with quick catalyst deactivation.
Drawings
FIG. 1 is a schematic flow diagram of one embodiment of a reaction apparatus for a multiphase reaction system.
FIG. 2 is a schematic flow diagram of a second embodiment of a reaction apparatus for a multiphase reaction system.
1-dispersed phase inlet; 2-a continuous phase inlet; 3-dispersed phase feeder; 4-a tube mixer; 5-an equal diameter riser reactor; 6-catalyst discharge port; 7-upper section of external circulation pipe; 8-liquid-solid separator; 9-lower section of external circulation pipe; 10-clear liquid outlet; 11-a catalyst inlet; 12-backwash liquid inlet; 13-liquid separator; 14-an aqueous phase outlet; 15-oil phase outlet; 16-product separation system.
Detailed Description
The following detailed description of embodiments of the utility model refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
A reaction device for a multiphase system comprises a riser reactor 5 with equal diameter, a liquid-solid separator 8, a liquid-liquid separator 13 and a tubular mixer 4, wherein the bottom of the riser reactor is provided with a dispersed phase inlet 1 and a catalyst discharge outlet 6, the top of the reactor is communicated with the inlet of the solid-liquid separator through an external circulation pipe 7, the intercepted liquid outlet of the solid-liquid separator is communicated with the bottom of the reactor through the tubular mixer, the clear liquid outlet 10 of the solid-liquid separator is communicated with the inlet of the liquid-liquid separator, the liquid-liquid separator is provided with a water phase outlet and an oil phase outlet, and the water phase outlet or the oil phase outlet is communicated with the inlet of the tubular mixer 4.
Preferably, the bottom of the reactor is also provided with a circulating material inlet, and the inlet of the tubular mixer is provided with a continuous phase inlet.
Preferably, the reactor is divided into a tube side and a shell side, the upper end and the lower end of the shell side are respectively provided with a heat exchange medium inlet and a heat exchange medium outlet, the tube side provides a reaction space for reaction materials, and the shell side is introduced with a heat exchange medium to control the temperature.
Preferably, the disperse phase inlet is provided with a disperse phase feeder 3 which is a porous pipe, a sintered metal pipe, an inorganic membrane pipe or an atomizing nozzle.
Preferably, the liquid-solid separator is a filtering assembly, the filtering assembly comprises a shell and a filtering pipe, and the filtering pipe is one or a combination of several of an inorganic ceramic membrane, a metal pipe membrane, a metal screen and a metal sintering pipe.
Preferably, the liquid-solid separator shell is also provided with a catalyst feeding port.
Preferably, in the liquid-solid separator, a back-flushing pipeline is arranged on the filtering component.
Preferably, the number of the external circulation pipes is one or more, wherein the part communicated between the outlet of the reactor and the liquid-solid separator is the upper section of the external circulation pipe, and the part communicated between the outlet of the trapped liquid of the liquid-solid separator and the tubular mixer is the lower section of the external circulation pipe.
Preferably, the diameter ratio of the external circulation pipe to the reactor is (0.3-3): 1, more preferably (0.5 to 2): 1.
preferably, the tubular mixer is an injection mixer, wherein the lower section of the circulating pipe is communicated with a main fluid inlet of the injection mixer, and a water phase outlet of the liquid-liquid mixer is communicated with a high-speed jet fluid inlet of the injection mixer.
The liquid-liquid separator is selected from one or the combination of a gravity settling tank, an oil-water coalescence separator and a fiber membrane surface separator.
In the reaction device for the multiphase system, the top of the reactor is provided with a mixed material outlet, and the bottom of the reactor is preferably provided with a dispersed phase inlet, a circulating material inlet and a catalyst discharge outlet respectively.
In the reaction device for the multiphase system, the disperse phase inlet is provided with a disperse phase feeder, the disperse phase can be an oil phase or a water phase, and the disperse phase feeder is a porous pipe, a sintered metal pipe, an inorganic membrane pipe or an atomizing nozzle. The dispersed phase feeder has a remarkable throttling effect, and the optimal range of the pressure difference between the front and the back of the feeder is required to be 0.05-3.0 MPa, and the liquid flow rate of a feeding port is 5-40 m/s.
In the reaction device for the multiphase system, one or more external circulation pipes are provided, one end of each external circulation pipe is connected with the mixed material outlet at the top end of the reactor, and the other end of each external circulation pipe is connected with the bottom of the reactor to form a circulation loop. Wherein, the upper section of the external circulation pipe is communicated between the top end of the reactor and the liquid-solid separator, and the lower section of the external circulation pipe is communicated between the solid-liquid separator and the circulating material inlet at the bottom of the reactor. Preferably, the inner diameters of the upper section of the external circulation pipe and the lower section of the external circulation pipe are the same, and the diameter ratio of the external circulation pipe to the reactor is (0.3-3): 1, preferably (0.5-2): 1.
the liquid-solid separator is preferably a filter assembly for liquid-solid separation of the material from the top of the reactor. The filter component comprises a shell and a filter pipe, wherein the filter pipe is selected from one or a combination of several of an inorganic ceramic membrane, a metal pipe membrane, a metal screen mesh, a metal sintering pipe and the like. The filter components can be one or more groups. The filtration assembly is provided with a clear liquid outlet and a trapped liquid outlet, the clear liquid outlet is communicated with the liquid-liquid separator, the trapped liquid outlet is communicated with the bottom of the reactor through the lower section of the downcomer, and the trapped liquid is used as a circulating material and returns to the bottom of the reactor through the jet mixer in the use process.
The liquid-solid separator can adopt a cross-flow filtration or dead-end filtration mode, when the cross-flow filtration is adopted, the liquid-solid separation unit is preferably arranged on the external circulation pipe, and the external circulation pipe is divided into an upper section of the external circulation pipe and a lower section of the external circulation pipe; when a dead-end filtration mode is adopted, the liquid-solid separation unit is optionally arranged at the top end of the external circulation pipe, and the intercepted materials return to the bottom of the reactor through the external circulation pipe by means of gravity. Preferably, the catalyst introduction port is provided on the filter assembly housing.
The filter assembly is provided with a filter backwash inlet, and a preferable backwash inlet pipeline and a clear liquid outlet pipeline obtained by liquid-solid separation share one interface on the shell of the filter assembly. The backwash liquid is selected from the group consisting of a filtered supernatant or a fresh feed solution.
In the reaction device for the multiphase system, the lower section of the external circulation pipe is communicated with the tubular mixer, and preferably a jet mixer is adopted. The recycled material from the retentate outlet of the liquid-solid separator is used as the main fluid of said jet mixer, and the feed from the continuous phase inlet and the recycled liquid phase from the continuous phase outlet of the liquid-liquid separator are used as high velocity jet fluids. The two materials are mixed by a jet mixer and then enter the bottom of the reactor.
In the application process of the reaction device for the multiphase system, the adopted catalyst is preferably a spherical catalyst with the particle diameter of 0.05-3.0 mm, and the spherical catalyst is added into the reaction device through a catalyst adding port arranged on a liquid-solid separator. As the abrasion and the inactivation of a part of catalyst are inevitably caused in the reaction process, in order to ensure the overall activity of the catalyst, the activity and the abrasion condition of the catalyst need to be regularly inspected, and a part of catalyst is discharged from a catalyst discharge outlet at the bottom of a straight pipe section of the reactor, so that the online updating of the catalyst is realized, and the influence on the operation period of the device caused by the shutdown of the device is avoided.
The application method of the utility model is illustrated by taking an oil phase raw material as a dispersed phase as an example, the water phase raw material is introduced from a continuous phase inlet, the oil phase raw material enters a reactor from the bottom through a dispersed phase inlet and a dispersed phase feeder, and a reactant flow flows upwards in a cylindrical reactor with equal diameter and generates multiphase contact reaction. The reaction material flow at the top of the reactor enters the upper section of the external circulation pipe and enters the liquid-solid separator for solid-liquid separation, the slurry flow containing catalyst particles is discharged out of the liquid-solid separator and enters the tubular mixer through the lower section of the external circulation pipe to be mixed with the water phase raw material from the continuous phase inlet and the circulating material at the water phase outlet of the liquid-liquid separator and then enters the bottom of the reactor; and clear liquid separated from the liquid-solid separator enters the liquid-liquid separator through a clear liquid outlet to separate an oil phase from a water phase, the separated oil phase is extracted through an oil phase outlet and further separated to obtain a product, and the separated water phase returns to the tubular mixer through a water phase outlet to be recycled.
The following further describes the embodiments and application methods of the present invention with reference to the drawings.
FIG. 1 is a schematic flow diagram of one embodiment of a reaction apparatus for a multiphase system. As shown in the attached figure 1, the reaction device for the multiphase system provided by the utility model comprises a lifting tubular reactor 5 with equal diameter, a liquid-solid separator 8, a liquid-liquid separator 13 and a tubular mixer 4, wherein the bottom of the reactor is provided with a dispersed phase inlet 1 and a catalyst discharge outlet 6, the dispersed phase inlet is provided with a dispersed phase feeder 3, and the tubular mixer adopts a jet mixer. The top of the reactor is communicated with the bottom of the reactor through an upper section 7 of an external circulation pipe, a solid-liquid separator 8, a lower section 11 of the external circulation pipe and a jet mixer in sequence, a clear liquid outlet 10 of the solid-liquid separator is communicated with an inlet of a liquid-liquid separator 13, a water phase outlet of the liquid-liquid separator 13 is communicated with a high-speed jet liquid inlet of the jet mixer, and the liquid-liquid separator is also provided with an oil phase outlet 15.
The embodiments of the present invention will be further described by taking the oil phase as the dispersed phase. A certain amount of catalyst is transferred into the equal-diameter riser reactor 5 in advance, a water phase raw material serving as a continuous phase enters the equal-diameter riser reactor 5 from a continuous phase inlet 2, a certain amount of oil phase raw material enters the equal-diameter riser reactor 5 from a dispersed phase inlet 1 through a dispersed phase feeder 3, and the dispersed phase feeder 3 is selected from a perforated pipe, a sintered metal pipe or an atomizing nozzle. In order to achieve a good dispersion effect and ensure good circulation flow in the reactor, the pressure drop of the dispersed phase feeder 3 is required to be 0.05-3.0 MPa, and the initial liquid flow rate at the outlet of the dispersed phase feeder reaches 5-40 m/s. After reaction, the material is extracted from the top of the equal-diameter lifting pipe type reactor 5 and enters an external circulation pipe 7, and liquid-solid separation is carried out in a liquid-solid separator 8 arranged at the middle section of the external circulation pipe. The liquid-solid separator 8 is preferably a filter assembly comprising a housing and a filter tube. The mixed material is subjected to cross flow filtration on the filtering component, a back washing medium inlet 12 is arranged at a clear liquid outlet, and when catalyst particles on the filtering pipe are excessively accumulated, back washing is carried out on the particles accumulated on the filtering pipe by using back washing material flow, so that the back washing period of the filtering pipe is favorably prolonged. Optionally, when the pressure difference between the two sides of the filter pipe is more than 0.2MPa, the filter pipe must be backwashed, so that the permeability of the filter pipe is recovered. The backwash inlet 12 preferably shares a common port with the filtered supernatant outlet 10. The backwash liquid is selected from the group consisting of a filtered supernatant or a fresh feed solution. The liquid trapped by the filtering component is used as a circulating material and is mixed with continuous phase feeding material by a jet flow jet mixer 4 and then enters the bottom of a riser reactor 5 with the same diameter. The circulating material is used as suction fluid, the continuous liquid phase feeding is used as high-speed jet fluid, the continuous liquid phase comprises fresh continuous phase feeding and a circulating liquid phase 14 of a liquid-liquid separation unit, and the jet flow velocity is preferably 3-30 m/s to ensure good mixing effect.
The filtered clear liquid enters a liquid-liquid separator 13 through an outlet 10. The liquid-liquid separator 13 is mainly used for separating oil phase and water phase, and can be a conventional gravity settling tank, an oil-water coalescence separator, a fiber membrane surface separator and a combination thereof. Wherein the separated rich products are extracted through an oil phase outlet 15 and are further separated, and the separated water phase circulation flow returns to the bottom of the reactor through a water phase outlet 14 and a jet flow jet mixer for recycling.
The catalyst is preferably spherical, the particle diameter is 0.05-3.0 mm, the catalyst feeding port is preferably arranged on the liquid-solid separator 8, and the catalyst can be added into trapped fluid and enters the reactor through an external circulation pipe. The catalyst discharge port is arranged at the bottom of the equal-diameter riser reactor 5. As abrasion and inactivation of a part of catalyst are inevitably caused in the reaction process, in order to ensure the overall activity of the catalyst, the activity and abrasion condition of the catalyst need to be regularly checked, a part of catalyst is discharged from a discharge outlet according to the condition, and a part of fresh catalyst is supplemented, so that the online updating of the catalyst is realized, and the influence on the operation period of the device caused by the shutdown of the device is avoided.
FIG. 2 is a schematic flow diagram of a second embodiment of a reaction apparatus for a multiphase reaction system. Unlike the attached FIG. 1, the reactor is divided into a tube side I and a shell side II by a tube wall, and the tube side and the shell side are not communicated. The upper end and the lower end of the shell pass are respectively provided with a heat exchange medium inlet 20 and a heat exchange medium outlet 21, wherein the tube pass provides a reaction space for reaction materials, and the shell pass is introduced with a heat exchange medium to exchange heat with the reaction materials in the tube pass so as to control the reaction temperature. The oil phase separated by the liquid-liquid separator 13 returns to the bottom of the reactor through an oil phase outlet 15 for circular reaction, and the separated water phase enters a product separation system 16 through a water phase outlet 14 for further separation.
The following examples further illustrate embodiments of the reactor apparatus for multiphase systems according to the utility model, without limiting the utility model thereto.
The example illustrates the effect of the reaction apparatus for multiphase reaction system provided by the present invention, wherein the purity of the raw material propylene is greater than 99.6%, and the titanium silicalite molecular sieve catalyst is adopted under the brand name HTS (the company engineerings in the south of the lake). The hydrogen peroxide is commercially available, the concentration of the hydrogen peroxide is 30 percent, and the concentration of the residual hydrogen peroxide adopts KMnO4Titration and product composition were analyzed by gas chromatography.
Example 1
The embodiment adopts a reaction device and a process shown in figure 1, wherein a mixed solution composed of hydrogen peroxide and methanol is used as a dispersed phase, the molar ratio of the methanol to the hydrogen peroxide is 2.0, the molar ratio of a fresh propylene feed to the hydrogen peroxide is 1.5, and the diameter of catalyst particles is 10-200 mu m. The reactor contains 3 uniformly distributed round tubes as tube passes, the bottom of each round tube corresponds to a dispersed phase feeder, the top end of each dispersed phase feeder is a 6mm sintered metal tube, the average pore diameter of each sintered metal tube is 7 mu m, the three dispersed phase feeders are connected with the dispersed phase feeding tubes through circular tubes, and the total pressure drop of the feeders is 0.25 MPa. The external circulation pipe is provided with a metal sintering pipe filtering component, and the average filtering pore diameter is 6 mu m. The liquid-solid mixture at the interception side of the filtering component circularly returns to the reactor, the filtrate extracted by the filtering component enters a gravity settling tank for liquid-liquid separation, the upper oil phase obtained by separation returns to the reactor, and the lower water phase is extracted for product separation and analysis.
The temperature of a reaction inlet is 45 ℃, the temperature of a reactor outlet is controlled to be 68 ℃ by introducing cooling water into a reactor shell, the pressure of a reaction part is 1.2MPa, and the apparent residence time of reaction materials in the reactor is 1.0 h.
The conversion rate of hydrogen peroxide obtained by sampling, analyzing and calculating the reaction result is more than 96 percent, and the selectivity of propylene oxide is 95 percent.
Wherein the conversion rate of the hydrogen peroxide is the ratio of the amount of the hydrogen peroxide consumed in the reaction to the amount of the hydrogen peroxide added. The propylene oxide selectivity is the ratio of the amount of the material that generates propylene oxide to the amount of the material that consumes hydrogen peroxide.
Claims (10)
1. The reaction device for the multiphase system is characterized by comprising an equal-diameter riser reactor (5), a liquid-solid separator (8), a liquid-liquid separator (13) and a tubular mixer (4), wherein the bottom of the riser reactor is provided with a dispersed phase inlet (1) and a catalyst discharge outlet (6), the top of the reactor is communicated with the inlet of the solid-liquid separator through an external circulation pipe (7), a trapped liquid outlet of the solid-liquid separator is communicated with the bottom of the reactor through the tubular mixer, a clear liquid outlet (10) of the solid-liquid separator is communicated with the inlet of the liquid-liquid separator, the liquid-liquid separator is provided with a water phase outlet and an oil phase outlet, and the water phase outlet or the oil phase outlet is communicated with the inlet of the tubular mixer (4); the equal-diameter riser reactor is divided into a tube side and a shell side, the upper end and the lower end of the shell side are respectively provided with a heat exchange medium inlet and a heat exchange medium outlet, the tube side provides a reaction space for reaction materials, and the shell side is introduced with a heat exchange medium to control the temperature.
2. The reactor according to claim 1, wherein the bottom of the reactor is further provided with an inlet for a circulating material, and the inlet of the tubular mixer is provided with an inlet for the continuous phase.
3. Reactor device for multiphase systems according to claim 1, characterized in that the disperse phase inlet (1) is provided with a disperse phase feeder (3) which is a perforated pipe, a sintered metal pipe, an inorganic membrane pipe or an atomizing nozzle.
4. The reaction device for the multiphase system according to claim 1, wherein the liquid-solid separator is a filter module, the filter module comprises a shell and a filter pipe, and the filter pipe is one or a combination of several of an inorganic ceramic membrane, a metal pipe membrane, a metal screen and a metal sintered pipe.
5. A reactor device for multiphase systems according to claim 4, wherein the housing of the liquid-solid separator is further provided with a catalyst inlet.
6. A reactor for multiphase systems according to claim 4, wherein the liquid-solid separator is provided with a back-flushing line on the filter module.
7. A reactor assembly according to any one of claims 1 to 6 wherein the external circulation pipe is one or more, wherein the upper section of the external circulation pipe is connected between the outlet of the reactor and the liquid-solid separator, and the lower section of the external circulation pipe is connected between the outlet of the liquid-solid separator and the tubular mixer.
8. The reactor according to claim 7, wherein the ratio of the diameters of the external circulation pipe and the reactor is (0.3-3): 1.
9. the reactor according to claim 1, wherein said tubular mixer is a jet mixer, wherein said lower section of said circulation tube is in communication with a main fluid inlet of said jet mixer, and wherein a water phase outlet of said liquid-liquid mixer is in communication with a high velocity jet fluid inlet of said jet mixer.
10. The reactor according to claim 1, wherein the liquid-liquid separator is selected from one or a combination of a gravity settling tank, a coalescer and a fiber membrane surface separator.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202120748028.9U CN216935945U (en) | 2021-04-13 | 2021-04-13 | Reaction device for multiphase system |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202120748028.9U CN216935945U (en) | 2021-04-13 | 2021-04-13 | Reaction device for multiphase system |
Publications (1)
Publication Number | Publication Date |
---|---|
CN216935945U true CN216935945U (en) | 2022-07-12 |
Family
ID=82288905
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202120748028.9U Active CN216935945U (en) | 2021-04-13 | 2021-04-13 | Reaction device for multiphase system |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN216935945U (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115197171A (en) * | 2021-04-13 | 2022-10-18 | 中国石油化工股份有限公司 | A kind of method and system for producing propylene oxide |
-
2021
- 2021-04-13 CN CN202120748028.9U patent/CN216935945U/en active Active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115197171A (en) * | 2021-04-13 | 2022-10-18 | 中国石油化工股份有限公司 | A kind of method and system for producing propylene oxide |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US6080372A (en) | Two stage reactor for continuous three phase slurry hydrogenation and method of operation | |
AU664429B2 (en) | Catalytic multi-phase reactor | |
CN100371309C (en) | Hydrogenation process of hydrogen peroxide fluidized bed by anthraquinone | |
CN102241558B (en) | Reaction device and process for preparing cyclohexene by selectively hydrogenating benzene | |
CN113368594B (en) | Liquid phase hydrogenation refining system device and method thereof | |
CN102051207A (en) | Method for enhancing mass transfer through suspension bed hydrogenation technology | |
CN101249405A (en) | Air-lift type circular current reactor | |
CN110961067B (en) | Continuous reaction device and method for benzoic acid hydrogenation | |
CN216935945U (en) | Reaction device for multiphase system | |
CN110003140B (en) | Device and method for synthesizing epichlorohydrin and regenerating catalyst on line | |
CN213160705U (en) | Olefin hydration reaction device | |
EP1392625B1 (en) | Process for separating liquid hydrocarbons from a particulate fischer-tropsch catalyst | |
EP1827646B1 (en) | System for facilitating transfer of a component from a liquid phase to a fluid phase | |
JPH0568869A (en) | Reaction method for suspended catalyst system | |
CN115197171A (en) | A kind of method and system for producing propylene oxide | |
CN112723989A (en) | Olefin hydration reaction method and system | |
CN111036148A (en) | A device and method for gas-liquid-solid reaction using microfoam packed bed | |
CA2027266A1 (en) | Liquid phase reaction process | |
CN202047018U (en) | Device for preparing cyclohexene from benzene through selective hydrogenation | |
CN204933428U (en) | A kind of paste state bed reactor | |
CN212999378U (en) | Immersed KMPR (KMPR) filtering complete device | |
CN101678299A (en) | Hydrogen-oxygen blender-distributor | |
CN222739122U (en) | A gas countercurrent liquid-solid descending bed reactor | |
CN215087001U (en) | Gas-liquid-solid three-phase continuous reaction device | |
CN105126710A (en) | Slurry bed reactor and application of slurry bed reactor in hydrogen peroxide production |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
GR01 | Patent grant | ||
GR01 | Patent grant |