CN207838958U - A kind of silicon carbide bed reactor - Google Patents

A kind of silicon carbide bed reactor Download PDF

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Publication number
CN207838958U
CN207838958U CN201820042374.3U CN201820042374U CN207838958U CN 207838958 U CN207838958 U CN 207838958U CN 201820042374 U CN201820042374 U CN 201820042374U CN 207838958 U CN207838958 U CN 207838958U
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China
Prior art keywords
silicon carbide
liquid phase
bed
shell
phase outlet
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Expired - Fee Related
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CN201820042374.3U
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Chinese (zh)
Inventor
白金
刘进博
张健
封瑞江
王海彦
龙文宇
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Liaoning Shihua University
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Liaoning Shihua University
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Abstract

The utility model is related to petrochemical industries, disclose a kind of silicon carbide bed reactor, liquid acid circulation pipe is respectively equipped in reactor shell(4), material inlet(5), gas phase outlet port(6)And liquid phase outlet port(7);It is vertically arranged microchannel reaction module and Froth separating member in shell successively from top to bottom(3);Material inlet(5)It is placed in case top;Liquid acid circulation pipe(4)Liquid acid feed inlet of the upper port through case top is communicated with housing cavity;Gas phase outlet port(6)Set on microchannel reaction module lower part.The utility model is using iso-butane and alkene as raw material, using liquid acid as catalyst, is alkylated and purpose product alkylate oil is obtained by the reaction.The utility model solves the problems, such as alkylation reactor, and temperature distribution is non-uniform, has the features such as feed distribution is good, temperature is easily controllable, and product quality is high.

Description

A kind of silicon carbide bed reactor
Technical field
The utility model belongs to petrochemical industry more particularly to a kind of silicon carbide bed reactor.
Background technology
It is alkylated at present to commercially produce in device, environmental pollution hidden danger, the activity of solid acid catalyst of hydrofluoric acid And ionic liquid solidification the problems such as blocking, restricts the popularizations of the relevant technologies, and sulfuric acid alkylation safety and operability it Between reached optimum balance.But there are reaction temperature height, acid hydrocarbon emulsifications to be not readily separated for the sulfuric acid alkylation technology of commercial Application, acid Consume the problems such as big.
CN205815148U discloses the device that a kind of sulfuric acid alkylation reaction product asks for flash evaporation, and filling is more in device The irregular micro- porous medium of layer, irregular micro- porous medium are semi-soft three-dimensional porous gauze packing, and dispersion is woven into fiber thread Composition, fiber thread are one or more in PTFE, PP, PE or glass fibre.The fiber thread compressed coefficient is larger in patent, influences The stability of device long-term operation, this outer fiber easy fracture, influences the product quality of alkylate oil.
CN103007853A discloses silicon carbide microchannel reactor and its application in preparing low-carbon olefin by hydrocarbon cracking, Microchannel is constituted filled with integral foam carbofrax material in reactor, it is outer to have metallic reactors shell.Integral foam is carbonized There is silicon materials the microchannel structure of three-dimensional foam, channel diameter range to produce low-carbon alkene in 0.1 ~ 2mm, for hydrocarbon cracking Hydrocarbon.Reactor is not provided with feed distributor in patent, and silicon carbide channel diameter is larger, if being used for liquid acid alkylation process, Sour hydrocarbon two-phase cannot be sufficiently mixed, and conversion ratio is too low.
Therefore, how micro passage reaction is advanced optimized, with realize be precisely controlled reaction temperature profile, make be System safety and stability long-term operation is that those skilled in the art need the outstanding problem solved.
Utility model content
The utility model overcomes the shortcomings of the prior art place and provides a kind of energy-efficient, safety and environmental protection, mass transfer Heat transfer property is ideal, and purpose product octane number height is, it can be achieved that be precisely controlled the silicon carbide bed reactor of reaction temperature profile.
In order to solve the above technical problems, the utility model is realized in this way:
A kind of silicon carbide bed reactor, including shell;Liquid acid circulation pipe, feedstock are respectively equipped on the shell Mouth, gas phase outlet port and liquid phase outlet port;The housing cavity is vertically arranged microchannel reaction module and breaks successively from top to bottom Foam separating member;The material inlet is placed in case top;The liquid of the liquid acid circulation pipe upper port through case top Body acid feed inlet is communicated with housing cavity;The gas phase outlet port is set to microchannel reaction module lower part;The liquid phase outlet port Lower part set on gas phase outlet port, and it is corresponding with Froth separating member.
As a preferred embodiment, microchannel reaction module described in the utility model includes fiber bed and silicon carbide bed Layer;The fibre bed is placed on silicon carbide bed.
Further, silicon carbide bed described in the utility model is by normal pressure-sintered high-purity foam silicon carbon structured packing structure At bed specific surface area is 300 ~ 3000 m2/m3;Voidage is 0.35 ~ 0.9.
Further, fiber bed described in the utility model is woven by oxytalan material, and bed specific surface area is 100~1000 m2/L;Voidage is 0.4 ~ 0.85;Bed ratio of height to diameter is 0.1 ~ 0.5.
Further, Froth separating member described in the utility model includes shell, grid, liquid phase end tab, stalk, liter Tracheae and liquid phase outlet;The grid, liquid phase end tab and stalk are respectively placed in enclosure cavity;The grizzly level is set In enclosure cavity bottom;The liquid phase end tab is horizontally placed on grid;The liquid phase outlet is horizontally placed at liquid phase extraction On plate, and connect with liquid phase outlet port;The port of the stalk and liquid phase end tab vertical connection;The riser is located at Cover top portion, one port are communicated with shell inner cavity, and Open Side Down for another port.
Further, spaced apart in shell described in the utility model to be equipped with multiple microchannel reaction modules.
The alkylation reactor of the utility model uses carbofrax material as microchannel filler, improves conventional alkylation Temperature Distribution in reactor can effectively realize that cryogenic alkylation reacts, there is operating condition to mitigate, and reaction is easily controllable, The features such as product quality is high is, it can be achieved that energy-efficient, safety, low-carbon and the continuous production of environmental protection.Test result shows carbonization The alkylate oil octane number that silicon bed reactor generates is high, low-sulfur, aromatic-free and alkene.
Description of the drawings
The utility model is described in further detail with reference to the accompanying drawings and detailed description.The protection model of the utility model Enclose the statement for being not only limited to following content.
Fig. 1 is the utility model silicon carbide bed reactor structural schematic diagram.
Fig. 2 is the utility model Froth separating member structural schematic diagram.
In figure:1, fiber bed;2, silicon carbide bed;3, Froth separating member;4, liquid acid circulation pipe;5, feedstock Mouthful;6, gas phase outlet port;7, liquid phase outlet port;3-1, shell;3-2, grid;3-3, liquid phase end tab;3-4, stalk;3-5、 Riser;3-6, liquid phase outlet.
Specific implementation mode
As shown in Figure 1, silicon carbide bed reactor, including shell;It is characterized in that:It is respectively equipped with liquid on the shell Sour circulation pipe 4, material inlet 5, gas phase outlet port 6 and liquid phase outlet port 7;The housing cavity is vertically set successively from top to bottom Set microchannel reaction module and Froth separating member 3;The material inlet 5 is placed in case top;The liquid acid circulation pipe 4 Liquid acid feed inlet of the upper port through case top is communicated with housing cavity;It is answered set on microchannel plate the gas phase outlet port 6 Module lower part;The liquid phase outlet port 7 is set to the lower part of gas phase outlet port 6, and corresponding with Froth separating member 3.This practicality The novel microchannel reaction module includes fiber bed 1 and silicon carbide bed 2;The fiber bed 1 is placed in silicon carbide bed 2 On.Silicon carbide bed 2 described in the utility model is made of normal pressure-sintered high-purity foam silicon carbon structured packing, bed specific surface Product is 300 ~ 3000 m2/m3;Voidage is 0.35 ~ 0.9.Fiber bed 1 described in the utility model is woven by oxytalan material It forms, bed specific surface area is 100 ~ 1000 m2/L;Voidage is 0.4 ~ 0.85;Bed ratio of height to diameter is 0.1 ~ 0.5.Referring to Fig. 2 It is shown, Froth separating member 3 described in the utility model include shell 3-1, grid 3-2, liquid phase end tab 3-3, stalk 3-4, Riser 3-5 and liquid phase outlet 3-6;The grid 3-2, liquid phase end tab 3-3 and stalk 3-4 are respectively placed in shell 3-1 In cavity;The grid 3-2 is horizontally placed at shell 3-1 cavity bottoms;The liquid phase end tab 3-3 be horizontally placed at grid 3-2 it On;The liquid phase outlet 3-6 is horizontally placed on liquid phase end tab 3-3, and is connected with liquid phase outlet port 7;The stalk The port of 3-4 and liquid phase end tab 3-3 vertical connections;The riser 3-5 is located at the top of shell 3-1, one port and shell The inner cavities 3-1 communicate, and Open Side Down for another port.It is spaced apart in shell described in the utility model to be equipped with multiple microchannel plates Answer module.
The application method of above-mentioned silicon carbide bed reactor is using iso-butane and alkene as raw material, is catalysis with liquid acid Agent is alkylated and alkylate oil is obtained by the reaction.Work as diameter of the housing>When 2.5 m, reactor head is arranged liquid feedstock and is distributed Device.Alkene described in the utility model is C3~C5Alkene;The liquid acid is sulfuric acid.Isobutane and olefins described in the utility model Molar ratio is 3 ~ 10:1;The liquid acid and the volume ratio of alkene are 0.5 ~ 2:1;The alkene residence time is 1 ~ 30min, reaction temperature Degree is -3 ~ 3 DEG C.
The utility model foam silicon carbon is in three-dimensional network connectivity structure, has larger specific surface area, higher machinery Intensity, excellent heat transfer and excellent acid-alkali-corrosive-resisting performance.For the deficiency of current alkylation reactor, silicon carbide is used for reference Efficient mass-and heat-transfer performance, the utility model can be precisely controlled temperature of reactor distribution, realize energy-efficient, safety, low-carbon With the continuous production of environmental protection.
Setting fiber bed 1 in the utility model shell, fiber bed 1 is by the material with fiber densification hole shape structure Composition, can be the materials such as the organic polymers such as glass fibre, polyethylene or inorganic matter, corrosion-resistant, have the thin hydrocarbon performance of parent's acid. Fiber bed 1 is placed on silicon carbide bed 2, in the reactor mainly as the distributor and redistributor of sour hydrocarbon two-phase.It is fine Dimension 1 specific surface area of bed is 100 ~ 1000 m2/ L, voidage are 0.4 ~ 0.85, preferably 0.55 ~ 0.75, and bed ratio of height to diameter is 0.1~0.5.When reactor shell diameter>When 2.5 m, liquid feed distributor should be arranged in reactor head.
Setting silicon carbide bed 2 in the utility model shell, silicon carbide bed 2 are advised by normal pressure-sintered high-purity foam silicon carbon Whole filler is constituted, mainly as the reaction zone of alkylation process.Silicon carbide is polar solid, easily soaks and adsorbs, liquid with water Acid can be dispersed in silicon carbide very well, form sorrel.Raw material under the effect of gravity, flows through, in liquid acid from sorrel surface Alkylation process is completed under catalytic action.Silicon carbide has larger reference area, enhances the reaction of alkylation process Rate and mass transfer rate, silicon carbide have larger thermal coefficient, enhance the rate of heat transfer of alkylation process, remove in time anti- Heat, temperature of reactor is answered to be evenly distributed.Silicon carbide bed specific surface area is 300 ~ 3000 m2/m3, voidage is 0.35 ~ 0.9, excellent It is selected as 0.55 ~ 0.75.
It is shown in Figure 2, Froth separating member is set in the utility model shell, and Froth separating member is by shell 3-1, lattice Grid 3-2, liquid phase end tab 3-3, stalk 3-4, riser 3-5, liquid phase outlet 3-6 are constituted.Grid 3-2 is horizontally placed at shell The lowermost end of 3-1;Liquid phase end tab 3-3 not trepannings, are horizontally placed on grid 3-2;Liquid phase outlet 3-6 is horizontally placed at liquid phase On end tab 3-3;Stalk 3-4 is connected with liquid phase end tab 3-3, is vertically arranged;Riser 3-5 is vertically installed in shell 3- On 1, Open Side Down.Shell 3-1, grid 3-2, liquid phase end tab 3-3, stalk 3-4 are placed in hydrocarbon liquid phase space, riser The outlets 3-5 are placed in gas-phase space.Liquid hydrocarbon enters Froth separating member by grid 3-2 with bubble from the lower parts shell 3-1, passes through Bubble breaking when grid, the liquid acid that a small amount of liquid acid carried secretly in bubble is deposited to reactor bottom under gravity are empty Between;Liquid hydrocarbon continues up flowing with a small amount of gas by stalk 3-4, and when reaching at the top of stalk 3-4, liquid hydrocarbon is in gravity Liquid phase end tab 3-3 is flowed under effect, and is extracted through liquid phase outlet 3-6;A small amount of gas is discharged into anti-by riser 3-5 Answer the gas-phase space of device bottom.
It is shown in Figure 1, multiple fiber beds 1 and silicon carbide bed can be arranged alternately in the utility model reactor enclosure body 2, the specific quantity that connects is determined according to treating capacity and air speed.1 bottom of fiber bed and 2 top close proximity of silicon carbide bed, but Section of coming to nothing is arranged between 1 top in 2 bottom of silicon carbide bed and next fiber bed.
Shown in Figure 1, material inlet 5 and liquid acid feed inlet is arranged in the utility model case top, to avoid Excessive reaction occurs for fiber bed 1, and material inlet 5 is placed on liquid acid feed inlet;Section, the Froth of coming to nothing between bed detach Gas phase outlet port is respectively set at shell at the top of component riser 3-5, for regulating and controlling the distribution of the pressure in reactor;Shell bottom Liquid phase outlet port 7 and liquid acid outlet port, liquid phase outlet port 7 and the liquid phase outlet 3-6 phases in Froth separating member is arranged in portion Even, liquid acid outlet port is placed in reactor lowermost end.
The utility model reactor shell shape is preferably cylinder, and reactor is disposed vertically, and reaction process is with iso-butane It is that raw material is alkylated and alkylate oil is obtained by the reaction using liquid acid as catalyst with alkene, alkene C3~C5Alkene, preferably For butylene, liquid acid preferably sulfuric acid.The molar ratio of iso-butane and alkene is 3:1~10:1, sour hydrocarbon volume ratio is 0.5:1~2:1, alkene Hydrocarbon residence time is 1 ~ 30min, and reaction temperature is -3 ~ 3 DEG C.
Feedstock amount and liquid acid internal circulating load are by the Liquid level on top fibers bed 1, when level fluctuation, adjustment Material inlet valve opening, while adjusting by proportional controller the valve opening of sulfuric acid pipeloop, keep it is stable into Expect acid hydrocarbon ratio and tower top liquid level.Gas phase outlet port flow is controlled by outlet port temperature, when temperature fluctuation, adjustment gas phase extraction Mouth valve opening, changes the pressure of reactor, further adjusts the amount of vaporization of iso-butane, reaches and remove reaction heat, control reaction The purpose of device temperature.Liquid phase extracted amount is by the boundary position control of sour hydrocarbon two-phase, and when boundary is fluctuated position, adjustment liquid phase outlet port valve is opened Degree keeps stable sour hydrocarbon boundary position.
Referring to Fig.1, the application method of the utility model silicon carbide bed reactor, be using iso-butane and alkene as raw material, Using liquid acid as catalyst, it is alkylated and alkylate oil is obtained by the reaction.Sour hydrocarbon two-phase enters reactor according to a certain percentage, Since fiber bed 1 has the function of very strong radial distribution, after reactant and liquid acid are by fiber bed 1, uniformly to flowing down It is dynamic to enter silicon carbide bed 2.Since there is silicon carbide bed 2 prodigious specific surface area, sour hydrocarbon two-phase to be realized in silicon carbide Film contacts, and completes alkylated reaction, and reaction heat is removed in iso-butane gasification.Sour hydrocarbon two-phase in the sedimentation separation of reactor bottom space, Liquid hydrocarbon passes through Froth separating member by bubble breaking with bubble, after being detached with gas, is extracted out from liquid-phase outlet, into separation work Section.Liquid acid is detached in the settlement space of reactor bottom with hydrocarbon liquid phase, is extracted out from liquid acid outlet port, and is pumped from liquid through peracid Body acid entrance Returning reactor.
Embodiment 1 ~ 3
Using the reactor of structure as shown in Figure 1, using sulfuric acid as catalyst, it is alkylated reaction.
The molar ratio of iso-butane and alkene is 3 ~ 10:1;Sour hydrocarbon volume ratio is 0.5 ~ 2:1;Reaction mass is in reactor Residence time is 1 ~ 30 min.Reactor bottom pressure is 0 ~ 0.05 MPa, and reactor pressure decrease is 0 ~ 0.4 MPa.Reaction temperature Maintain -3 ~ 3 DEG C.
Structure of reactor is:Reactor diameter is 50 ~ 300 mm, is highly 250 ~ 2500 mm, and fiber bed height is 10 ~ 120 mm, silicon carbide bed height are 100 ~ 1500mm.
Specific reaction condition is shown in Table 1, and reaction result is shown in Table 2.
Comparative example 1 ~ 2
The horizontal mechanical stirred reactor that comparative example 1 is restrained using conventional inside setting refrigeration, comparative example 2 use fiber Module micro passage reaction, reaction condition is referring to table 1, and reaction result is referring to table 2.
1 embodiment of table and comparative example alkylated reaction essential condition
Above with respect to the specific descriptions of the utility model, it is merely to illustrate the utility model and is not limited to this practicality newly Technical solution described in type embodiment.It will be understood by those of ordinary skill in the art that still can to the utility model into Row modification or equivalent replacement, to reach identical technique effect.Needs are used as long as meeting, all in the protection domain of utility model It is interior.

Claims (6)

1. a kind of silicon carbide bed reactor, including shell;It is characterized in that:Liquid acid circulation pipe is respectively equipped on the shell (4), material inlet(5), gas phase outlet port(6)And liquid phase outlet port(7);The housing cavity is vertically set successively from top to bottom Set microchannel reaction module and Froth separating member(3);The material inlet(5)It is placed in case top;The liquid acid is followed Endless tube(4)Liquid acid feed inlet of the upper port through case top is communicated with housing cavity;The gas phase outlet port(6)Set on micro- Pathway reaction module lower part;The liquid phase outlet port(7)Set on gas phase outlet port(6)Lower part, and with Froth separating member(3) It is corresponding.
2. silicon carbide bed reactor according to claim 1, it is characterised in that:The microchannel reaction module includes fibre Tie up bed(1)And silicon carbide bed(2);The fiber bed(1)It is placed in silicon carbide bed(2)On.
3. silicon carbide bed reactor according to claim 2, it is characterised in that:The silicon carbide bed(2)By normal pressure It is sintered high-purity foam silicon carbon structured packing to constitute, bed specific surface area is 300 ~ 3000 m2/m3;Voidage is 0.35 ~ 0.9.
4. silicon carbide bed reactor according to claim 3, it is characterised in that:The fiber bed(1)By acidproof fibre Dimension material weaves, and bed specific surface area is 100 ~ 1000 m2/L;Voidage is 0.4 ~ 0.85;Bed ratio of height to diameter be 0.1 ~ 0.5。
5. silicon carbide bed reactor according to claim 4, it is characterised in that:The Froth separating member(3)Including Shell(3-1), grid(3-2), liquid phase end tab(3-3), stalk(3-4), riser(3-5)And liquid phase outlet(3-6); The grid(3-2), liquid phase end tab(3-3)And stalk(3-4)It is respectively placed in shell(3-1)In cavity;The grid(3- 2)It is horizontally placed at shell(3-1)Cavity bottom;The liquid phase end tab(3-3)It is horizontally placed at grid(3-2)On;The liquid phase Outlet(3-6)It is horizontally placed at liquid phase end tab(3-3)On, and with liquid phase outlet port(7)Connect;The stalk(3-4) Port and liquid phase end tab(3-3)Vertical connection;The riser(3-5)Positioned at shell(3-1)Top, one port with it is outer Shell(3-1)Inner cavity communicates, and Open Side Down for another port.
6. silicon carbide bed reactor according to claim 5, it is characterised in that:It is spaced apart in the shell to set There are multiple microchannel reaction modules.
CN201820042374.3U 2018-01-11 2018-01-11 A kind of silicon carbide bed reactor Expired - Fee Related CN207838958U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108126637A (en) * 2018-01-11 2018-06-08 辽宁石油化工大学 A kind of silicon carbide microchannel alkylation reactor and its application method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108126637A (en) * 2018-01-11 2018-06-08 辽宁石油化工大学 A kind of silicon carbide microchannel alkylation reactor and its application method
CN108126637B (en) * 2018-01-11 2023-10-13 辽宁石油化工大学 Silicon carbide microchannel alkylation reactor and application method thereof

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Granted publication date: 20180911

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