CN105498646B - The three-phase flow catalytic reaction method of reaction kettle and the application reaction kettle - Google Patents

The three-phase flow catalytic reaction method of reaction kettle and the application reaction kettle Download PDF

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Publication number
CN105498646B
CN105498646B CN201511027900.6A CN201511027900A CN105498646B CN 105498646 B CN105498646 B CN 105498646B CN 201511027900 A CN201511027900 A CN 201511027900A CN 105498646 B CN105498646 B CN 105498646B
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flow
guiding structure
reaction
permeable member
reaction kettle
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CN105498646A (en
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高麟
汪涛
樊彬
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Intermet Technology Chengdu Co Ltd
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Intermet Technology Chengdu Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • B01J8/006Separating solid material from the gas/liquid stream by filtration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/085Feeding reactive fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00893Feeding means for the reactants
    • B01J2208/00902Nozzle-type feeding elements

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The three-phase flow catalytic reaction method of reaction kettle and the application reaction kettle.The present invention is intended to provide the reaction kettle of high production efficiency, while the three-phase flow catalytic reaction method using the reaction kettle being provided;Being related to field is a kind of chemical reaction device field.To achieve the above object, reaction kettle provided by the invention, it include autoclave body, reaction chamber is equipped in autoclave body, it include flow-guiding structure in reaction chamber, the flow-guiding structure includes permeable member, wherein flow-guiding structure is communicated with inlet port and outlet port, or wherein flow-guiding structure includes the first flow-guiding structure and the second flow-guiding structure, first flow-guiding structure is connected to feed inlet, second flow-guiding structure is connected to discharge port, reactant enters reaction chamber by permeable member after being passed through from feed inlet and reacts, the discharge port discharge that obtained product is connected to by permeable member from flow-guiding structure.The present invention also provides a kind of three-phase flow catalytic reaction methods using aforesaid reaction vessel simultaneously.

Description

The three-phase flow catalytic reaction method of reaction kettle and the application reaction kettle
Technical field
Field of the present invention is a kind of chemical reaction device field more particularly to three-phase flow reaction field.
Background technique
In the prior art, it is reacted, and is utilized including liquid and gas substance in disperse system in chemical field The production reaction that solid-phase catalyst is catalyzed, what is generallyd use is two ways:
The first is to be fixed catalyst in a kettle, using in disperse system as catalyst carrier using fixed bed body Liquid and gas mixing after contact with catalytic bed realization catalysis react.
In this reaction kettle, the position of catalyst in a kettle is relatively fixed, the position of catalyst in a kettle It will not generally occur to disperse and mobile, thus ought be after the reaction was completed without considering will to be filtered between catalyst and product point From can also reduce the loss of catalyst.
But in this reaction kettle, it is provided with mechanical stirring equipment often to reinforce between reactant and catalyst Contact, but be located in fixed catalytic bed due to catalyst, so that the contacting efficiency of catalyst and reactant is still lower.
It is placed in reaction kettle in the form of solid granule using by catalyst for current second, in this way by catalyst It is dispersed in disperse system and is contacted with reactant.
In this reaction kettle, the position of catalyst in a kettle is relatively free, can disperse in a kettle And movement, so as to preferably realize the contact between catalyst and reactant.
But in this reaction kettle, often there are problems that two:
Be first it is still to be improved in the contacting efficiency in disperse system between reactant about catalyst, this is mainly Because the solid-phase catalyst in disperse system can settle under the effect of gravity, even if in the premise for being provided with mechanical stirring equipment Under, the concentration of solid-phase catalyst is often disperse system lower layer much larger than upper layer.This is because mixing plant can be under normal conditions It is accomplished that the substance contact for reinforcing same level in disperse system, and the substance for reinforcing being located in disperse system different level is connect Then effect is extremely limited for touching.
Secondly there is also a problem be exactly wait react complete after need to consider mistake between catalyst and product Filter separation problem.In the prior art, currently used is after completion of the reaction to carry out the substance export in reaction kettle again Filter.Structure is complicated for such production equipment, also increases the process in production, also adds the loss of product and catalyst Probability.Why there is such problems in the prior art, a reason first be exactly those skilled in the art not Designing a kind of suitable filter structure can install in a kettle while will not also be to equipment existing for script in reaction kettle It impacts;Secondly, the working environment in chemical reaction in reaction kettle generally has corrosivity, more badly, be difficult to find The work such as a kind of filter material can be filtered in operating condition severe in this way, the vibration of blowback and mechanical stirring and can transport steadily in the long term Row.
In summary as can be seen that being directed to three-phase flow catalytic reaction at present, lack a kind of ideal high efficiency production equipment With reaction production method.
Summary of the invention
The present invention is intended to provide a kind of reaction kettle of high production efficiency, while a kind of three-phase flow of application reaction kettle being provided Catalytic reaction method;
Secondly the present invention also provides the reaction kettles of another high production efficiency, while providing a kind of application reaction kettle Three-phase flow catalytic reaction method.
First of all for above-mentioned first purpose reaction kettle provided by the invention is realized, includes autoclave body, be equipped in the autoclave body Reaction chamber includes flow-guiding structure in the reaction chamber, which includes permeable member, and wherein flow-guiding structure is communicated with Inlet port and outlet port, reactant enter reaction chamber by permeable member after being passed through from feed inlet and react, the life that will be obtained The discharge port discharge being connected to by permeable member from flow-guiding structure at object.
In aforesaid reaction vessel, raw material is subjected to production reaction in reaction chamber, wherein being provided with water conservancy diversion knot in the reactor chamber Structure is connected to inlet port and outlet port, raw material can be passed through in reaction chamber by flow-guiding structure in this way, can also be by reaction chamber The middle obtained product that reacts is discharged by flow-guiding structure from discharge port.
It wherein include permeable member on flow-guiding structure, reactant is passed into reaction chamber from feed inlet and needs through the infiltration Saturating component;Product is also required to from discharge port discharge through the permeable member.
In this way, the parameters such as aperture, the porosity of permeable member can be selected according to needs of production first, from And interception separation can be carried out to substance specific in reaction kettle by reaching, and realize reaction and filtering integral.
Secondly, in above-mentioned reaction kettle, moreover it is possible to by the way that structure, the location and shape of flow-guiding structure in the reactor chamber are arranged, To carry out water conservancy diversion and mixing to the substance in reaction chamber using the flow-guiding structure.
Wherein the present invention in flow-guiding structure mainly have there are two advantage:
First, the contact area of different material in reaction kettle can be increased.Due to flow-guiding structure be connected to feed inlet, in this way from The raw material that feed inlet is passed through flow-guiding structure can be contacted by permeable member surface with another raw material in reaction chamber.From And the contact area of different material is increased, and then increase the reaction efficiency in reaction kettle between different material substance.
Second, it may be implemented to accelerate the mixing in reaction kettle between different material substance.From feed inlet by raw material with a constant speed Degree can form osmotic pressure after being passed through diversion cavity inside and outside permeable member, can thus pass through the hole of control permeability hole Diameter, porosity, while cooperating the speed of control throat-fed, and then realize and the raw material for being passed through diversion cavity is had into certain speed Enter reaction chamber by permeable member, similar churned mechanically function can be reached to raw material existing for script in reaction chamber in this way Effect, and according to hydrodynamics it is found that if the raw material in diversion cavity passes through permeable member with certain speed, also in reaction chamber Middle formation local turbulent.It is equivalent to lead to raw material from feed inlet using the permeability hole on permeable member in flow-guiding structure in this way After entering diversion cavity, by raw material with certain pressure dissipation to reaction chamber, while to another Central Plains being originally present in reaction chamber Material causes to stir.
And it is possible to be adjusted according to actual needs to the quantity of flow-guiding structure and distributing position, and to feed inlet It is equipped with certain speed, the solid matter same to disperse system is can be realized in this way and fluidizes, so-called fluidisation refers to disperse system In gas phase or liquid velocity reach one timing, gradually by solid matter hold up present suspended state.Such solid matter It is difficult the lower end that sedimentation is gathered in reaction chamber, and then realizes that solid matter is evenly dispersed in disperse system.
To which above-mentioned flow-guiding structure may be implemented to accelerate the mixing in reaction kettle between different material substance, and then improve reaction Efficiency.
In summary as can be seen that reaction kettle provided by the invention, mainly can from increase raw material contact area, accelerate it is former Expect mixing velocity, simplify the various aspects such as equipment and process and organically combine, to realize a kind of more high efficiency compared with prior art Consersion unit.
Further, the flow-guiding structure is tubular structure, wherein permeable member is located on tube wall.This is one kind to upper It states reaction kettle structure to be advanced optimized, permeability hole is opened up using the permeable member of tubular structure and on tube wall, it can be very Big degree increase raw material is contacted after being passed into flow-guiding structure from feed inlet with the substance in reaction chamber and mixed efficiency. And it is relatively uniform that extraneous stress acts on tubular structure surface, and tubular structure itself also adopt by large surface area, inventor's discovery It may be implemented that flow-guiding structure is more stable and efficient operation with the permeable member of tubular structure.
Further, the permeable member includes table body the first supporter of aperture, the permeable member further includes There is the filter material to fit with first supporter.This is a kind of preferably to be tied to the above-mentioned permeable member with permeability hole Structure.Fitting support is carried out to filter material using first supporter, to realize that flow-guiding structure has stable structure.
It is worth noting that in said structure, being bonded between the first supporter and filter material may include that there are two types of feelings Condition: being located at permeable member periphery one is filter material and be located at reaction chamber side, and there are also one is filter materials to be located at permeable member inner circumferential position In the side of diversion cavity.
Further, the permeable member is located at filter material is equipped with compressing member on one side;The compressing member is preferably surrounded on and leads Flow structure week body ring-shaped clip.Filter material is firmly located in the position to fit with the first supporter by compressing member realization It sets, the filter material on flow-guiding structure permeable member is not easy to deviate.Simultaneously also water conservancy diversion can be further strengthened by the compressing member Structural stability of the filter material in filtering or blowback work in structure.The compressing member is preferably wherein surrounded on flow-guiding structure The ring-shaped clip of all bodies is a kind of further preferred structure, can by flow-guiding structure week body several be parallel to each other is set Ring-shaped clip realizes that filter material positioning is more stable on flow-guiding structure, also can effectively reinforce the whole structural stability of flow-guiding structure.
It remarks additionally herein, due to hereinbefore it has been mentioned that being bonded between filter material and the first supporter can be with Comprising two kinds of situations, so the side that permeable member periphery is located at reaction chamber may also be arranged in the corresponding compressing member, The side that permeable member inner circumferential is located at diversion cavity may be set.
Further, the filter material uses a kind of flexible, porous metal foil.This is one to the filter material in filter element Preferably, flexible, porous metal foil described herein refers to the Chinese invention patent application that applicant formerly submits to kind The flexible, porous metal foil mentioned in 201410609038.9, it by solid solution alloy is base that this flexible, porous metal foil, which is a kind of, The thin slice that the metal polyporous material of body phase is constituted.The average pore size of such flexible, porous metal foil is 0.05~50 μm, hole Gap rate is 40%~70%, with a thickness of 1~100 μm.Filter material made of the flexible, porous metal foil has very high mistake Precision is filtered, while material porosity with higher itself can ensure that good osmotic efficiency, so that manufactured filter material can have Preferable filter effect.Also, described flexible, porous metal foil itself has the biggish strength of materials and toughness, manufactured filter Material can bear extraneous biggish pressure in flow-guiding structure.And the flexible, porous metal foil also have it is certain soft Property, corresponding shape and structure can be supported to be bonded with the first supporter according to the contour structures of flow-guiding structure.It can be seen that Select above-mentioned flexible, porous metal foil that can realize a kind of effect mutually shone between flow-guiding structure filter material in the present invention Fruit, to obtain a kind of permeation filtration effect preferably and the flow-guiding structure of stable structure.It is only needed at this time using in current technology Material processing technology, can also realize above-mentioned flexible, porous metal foil have stronger corrosion resistance and heat-resisting quantity, thus Can in high temperature or high corrosion operating condition long-term stable work.
Further, being equipped with the second supporter in the diversion cavity, connected between second supporter and permeable member There is floor.To be further supported inside diversion cavity to flow-guiding structure by second supporter, the branch Support mode is realized using the floor being connected between the second supporter and permeable member.
It preferably, include the porous hollow being axially arranged along tube body in the diversion cavity that the permeable member of tubular structure surrounds The second supporter of tubulose, and second supporter is connected to feed inlet, the second supporter Zhou Tiyu permeable member inner wall Between be equipped with several evenly spaced floors.Second supporter is set as porous hollow tubular structure, and by the hollow tubular knot Structure connect the raw material being passed into flow-guiding structure to avoid feed inlet with feed inlet and causes directly to impact to permeable member, especially The protection to filter medium structure more may be implemented when on permeable member including filter material, the second supporter is arranged to edge simultaneously Several evenly spaced floors are axially arranged in tube body, to effectively reinforce the overall stability of flow-guiding structure.
Further, the autoclave body in be equipped with several flow-guiding structures, wherein flow-guiding structure be located in reaction chamber respectively with Autoclave body upper and lower side is fixedly connected, wherein autoclave body be equipped with several mutually independent feed inlets and/or discharge port respectively with each water conservancy diversion knot Structure connection.Raw material contact area can be further increased by several flow-guiding structures first in this way, and by several flow-guiding structures The material mixing of variant position in reaction chamber can effectively be reinforced in the reactor chamber by setting up separately, to improve production efficiency.And Several flow-guiding structures are provided with to be separately connected with mutually independent feed inlet and/or discharge port, it so first can be according to production Actual needs individually opens or closes each flow-guiding structure setting valve, while being also beneficial to the maintenance, cleaning, inspection of equipment The operation such as repair.
It should be understood that above-mentioned several mutually independent feed inlets and/or discharge port respectively with each water conservancy diversion knot Structure connection is primarily to realize that can carry out individual charging control and/or discharging control to each flow-guiding structure (cooperates corresponding Control valve), and the flow-guiding structure of upstream connect with to(for) each mutually independent feed inlet, each discharge port are connect with flow-guiding structure Downstream inlet port and outlet port can then be crossed and carry out raw material or finished product conveying for trunk access.
Further, the autoclave body lower end or close lower end are equipped with inlet port and outlet port, middle charging aperture and discharging Mouth is connected to for two parallel branches with flow-guiding structure.It is excellent with flow-guiding structure connection type that this is a kind of pair of inlet port and outlet port It selects, and when pan feeding substance and discharging substance are two kinds of not homomorphisms of gas and liquid, are especially suitable for using above-mentioned and be coupled Structure.Because being less likely to occur composite pollution between raw material and finished product, and will when pan feeding substance and discharging substance are not homomorphism Inlet port and outlet port parallel connection is connect with flow-guiding structure again for two branches can make the overall structure of reaction kettle more compact, It can also realize the effect of blowback to the permeable member on flow-guiding structure by pan feeding and the process of discharging simultaneously.
In summary as can be seen that reaction kettle provided by the invention, can mainly contact from accelerating to produce raw material in reaction Area, raw material mixing velocity simplify the combination of the various aspects such as equipment and process, to realize one kind compared with prior art more Efficient consersion unit.
Meanwhile the present invention is to provide a kind of three-phase flow catalytic reaction methods using aforesaid reaction vessel.The reaction kettle It include the reaction chamber for containing material liquid, and reaction kettle includes feed inlet for being passed through unstripped gas and for discharge liquor The discharge port of body product;First by material liquid be placed in reaction chamber in, solid catalyst is placed in reaction chamber, from feed inlet to It is passed through unstripped gas in reaction chamber, to close feed inlet after the reaction was completed, opens discharge port and exports liquid product.Above-mentioned three Flow catalytic reaction method is a kind of method carried out using reaction kettle provided in the present invention.In the above-mentioned methods, in reaction chamber In contained raw material liq, and need to be passed through unstrpped gas into reaction chamber, by between raw material liq and unstrpped gas It is mixed, under the catalysis of solid catalyst, realization converts the feedstock to finished industrial product.Here it is the three-phase flow (examples If above-mentioned raw material is liquids and gases, catalyst is solid) catalysis reaction.
But in current technology, what is generallyd use is the lower bottom end position that solid catalyst is placed on to reaction kettle, To avoid too dispersing in the disperse system of catalyst in a kettle, cause after the reaction was completed to purify the filtering of product The problems such as cost increases, and catalyst attrition increase and the contaminated risk of catalyst is also be easy to cause to increase.So current skill What is generally taken in art is the bottom position prevented solid catalyst in reaction kettle.
Certainly, those skilled in the art also attempted to disperse solid catalyst in disperse system to increase contact catalysis Efficiency, but those skilled in the art have found that, even if being provided with mixing plant in disperse system, solid matter is existed by graviational interaction It can still be settled in disperse system, by mixing plant it is achieved that same level by solid matter in disperse system Mixing of advancing disperses, and for being stirred position of the solid matter out of disperse system close to lower part in disperse system The position on top, then it is opposite to be not easily accomplished.
And in method provided by the invention, can not need to increase additional mixing plant also can by solid catalysis object compared with Dispersion mixing is into reaction kettle in disperse system well, at the same be also able to achieve solid catalyst and reaction product are carried out it is good Separation.To realize a kind of efficient three flow catalytic reaction methods.
The principle that method provided in the present invention has the above advantages is to have contained liquid charging stock in autoclave body in reaction chamber, And solid catalyst is placed in reaction chamber, is passed through unstripped gas into reaction kettle from feed inlet by flow-guiding structure.In this way, first It first can be by the parameter of permeability hole on permeable member in control flow-guiding structure, so that gas is passing through permeability hole on permeable member While also result in gas velocity of liquid assets slowed down, as the gas velocity that feed inlet is passed through flow-guiding structure increases, gas The amount assembled in flow-guiding structure also gradually increases, and also gradually increases from the air pressure in flow-guiding structure in diversion cavity accordingly Add, at this moment, pressure is discharged into material liquid by the unstripped gas that permeability hole enters in reaction chamber from diversion cavity, thus sharp The material liquid in reaction chamber is stirred with gas realization is passed through into reaction chamber from flow-guiding structure, is accomplished that first in this way Uniform mixing between unstripped gas and material liquid.And it can also be by the shape of flow-guiding structure, position, quantity in reaction kettle Press down or be the modes such as parameter that permeability hole is set, may be implemented to exist solid catalyst according to hydrodynamics in the prior art What is mixed in reaction chamber is relatively uniform.
Simultaneously in the above-mentioned methods, after reacting completion, the product that reaction is generated is discharged by discharge port to react Kettle, at this point, recycling the permeability hole in flow-guiding structure on permeable member that the catalyst of solid phase in disperse system is isolated to realize Drain and filtering integral operation are realized in the reactor chamber.
In summary as can be seen that three-phase flow catalytic reaction method provided by the invention, can effectively improve catalysis reaction Contact area between middle raw material can improve raw material mixing velocity, can be realized coming into full contact with for catalyst and reactant, and And it can enough realize the operation of drain filtering integral, while also simplifying production equipment and process.Three in the present invention Flow catalytic reaction method realizes the combination of above-mentioned advantage, to be a kind of catalysis more efficient compared with the existing technology Reaction method.
Secondly, this includes autoclave body the present invention also provides a kind of reaction kettle of high production efficiency, reaction is equipped in the autoclave body Chamber includes flow-guiding structure in the reaction chamber, which includes permeable member, and wherein flow-guiding structure includes first Flow-guiding structure and the second flow-guiding structure, first flow-guiding structure are connected to feed inlet, and second flow-guiding structure is connected to out Material mouth, reactant enter reaction chamber by permeable member after being passed through from feed inlet and react, and obtained product is passed through infiltration The discharge port discharge that saturating component is connected to from flow-guiding structure.
Reaction kettle belongs to a total inventive concept in such reaction kettle and above-mentioned first, has several cross-correlation The technical characteristic of connection, wherein flow-guiding structure includes the first flow-guiding structure and the second flow-guiding structure, wherein first water conservancy diversion Fabric connectivity feed inlet, the second flow-guiding structure is connected to discharge port, to realize the reaction work of reaction kettle.
Meanwhile three above-mentioned flow catalytic reaction methods are applied equally to second of reaction kettle provided by the invention.
Below with reference to illustrate the drawings and specific embodiments in the present invention reaction kettle and application the reaction kettle three Phase flow catalytic reaction method is further described and illustrates.
Detailed description of the invention
Fig. 1 is the reaction kettle in embodiment one.
Fig. 2 is flow-guiding structure radial section cutaway view Amplified image in reaction kettle in embodiment one.
Fig. 3 is flow-guiding structure axial cross section cutaway view Amplified image in reaction kettle in embodiment one.
Fig. 4 is the reaction kettle in embodiment two.
Wherein, in Figure of description, the corresponding relationship of each label and structure is successively are as follows:
1 is autoclave body, and 12 be reaction chamber, and 21 be feed inlet, and 22 be discharge port, and 3 be flow-guiding structure, and 3a is the first water conservancy diversion knot Structure, 3b are the second flow-guiding structure, and 30 be the permeable member of flow-guiding structure, and 301 be the first supporter, and 302 be filter material, and 31 be the Two supporters, 32 be floor, and 33 be ring-shaped clip, the steady brace of 4 flow-guiding structures.
Specific embodiment
Embodiment one is as shown in Figure 1 to Figure 3.
As shown in Figure 1, reaction kettle in example 1 includes autoclave body 1, which surrounds inside by shell and has The structure of cavity, the cavity in autoclave body 1 are reaction chamber 12.
The wherein lower bottom end position of autoclave body 1 is connected with several feed inlets independent of each other 21 and discharge port 22.And it is each It is arranged independently of one another between feed inlet 21, between each discharge port 22, certainly, 21 upstream of each feed inlet is connected with one jointly The trunk access of a feedstock transportation, correspondingly, 22 downstream of each discharge port is connected with the trunk of finished product conveying jointly Access.
Meanwhile in example 1, the water conservancy diversion knot of several vertical tubular structures is laid in the reaction chamber 12 in autoclave body 1 Structure 3.
In example 1 as Fig. 1 can be seen that each individual feed inlet 21 with a discharge port 22 in autoclave body 1 Bottom be in parallel, feed inlet 21 and discharge port 22 are intersected in the position connecting with flow-guiding structure 3 after parallel connection is two branches. That is, each flow-guiding structure 3 is connected with a feed inlet 21 and a discharge port 22, and the feed inlet 21 It is connected in parallel to each other with feed inlet 21.To need to be provided with naturally between above-mentioned flow-guiding structure 3 and feed inlet 21 and discharge port 22 Corresponding flow valve or direction valve realize control.
In said structure, it is parallel to each other and puts between the flow-guiding structure 3 of several tubular structures in the reaction chamber 12 It sets, in example 1, each flow-guiding structure 3 is fixed on evenly and at intervals in reaction chamber 12, and the tubulose knot of flow-guiding structure 3 More than the vertical highly preferred half for the vertical height of reaction chamber 12 of structure, in example 1, the flow-guiding structure 3 is managed Shape structure length reaches 2/3rds or more of 12 inner height of reaction chamber in reaction chamber 12.
In addition, the flow-guiding structure 3 lower end in reaction chamber 12 passes through the junction with feed inlet 21 and discharge port 22 It is fastenedly connected with the realization of autoclave body 1, while in the top position of autoclave body 1, is provided with the fixed drawing being correspondingly arranged with each flow-guiding structure 3 Bar 4 is connected to 3 upper end of flow-guiding structure using the steady brace 4, in this way to realize that the flow-guiding structure 3 of tubular structure is reacting Upper and lower ends in chamber 12 position fastening.
Again as shown in Figures 2 and 3, flow-guiding structure 3 in example 1 is using cylindrical tube structure, the tubulose knot Structure includes the permeable member 30 of hollow cylinder structure, and the hollow cavity which surrounds is leading in flow-guiding structure 3 Flow chamber.
Also, the permeable member 30 includes that table body gathers the first supporter 301 and filter material 302 of several apertures. Both the filter material 302 and the first supporter 301 are bonded to each other, and the first supporter 301 provides support to filter material 302.Wherein, In example 1,30 periphery of permeable member is located at after the filter material 302 is bonded with the first supporter 301 by reaction chamber 12 Side.Simultaneously in example 1, it can be pasted after first supporter 301 and filter material 302 are bonded in the two It is provided with cementing or pad or face between conjunction face to realize the sealed connection of material between the two, and then further strengthens two Fitting intensity between person.
In addition, as shown in figure 3, tubular structure flow-guiding structure 3 close to side week on body of filter material 302, if being provided with The dry ring-shaped clip 33 being parallel to each other carries out filter material 302 to surround compression.
In example 1, the filter material 302 is using a kind of flexible, porous metal foil, the flexible, porous metal foil It is the flexible, porous metal foil mentioned in Chinese invention patent application 201410609038.9 that applicant formerly submits, it is this soft Property multicellular metal foil is a kind of thin slice being made of solid solution alloy the metal polyporous material of matrix phase.Such flexibility is more The average pore size of mesoporous metal foil is 0.05~50 μm, and porosity is 40%~70%, with a thickness of 1~100 μm.The flexibility is more Filter material 302 made of mesoporous metal foil has very high filtering accuracy, while material porosity with higher itself can ensure that Efficient osmotic efficiency, so that manufactured filter material 302 can have preferable filter effect.And this flexible, porous metal foil sheet Body is metal material, can intensity with higher, itself also have certain ductility and toughness, can be very good to be coated on On first supporter 301, in example 1, the flexible, porous metal foil is coated on the tube wall of the first supporter 301 After the two fits, can the lap-joint of flexible, porous metal foil carry out welding or it is cementing, will be filtered so as to realize Material 302 is stable to be fitted on the first supporter 301, and is connect in filter material 302 with 302 lap-joint's forming face of filter material, and face connects The place of connecing may insure junction uniform force, stable connection using cementing or welding.
At the same time, the stable structure for further strengthening flow-guiding structure 3 in embodiment one, in flow-guiding structure 3 It is provided with the second supporter 31 of hollow tubular in diversion cavity, is provided on 31 tube body of the second supporter of the hollow tubular several Through-hole.Second supporter 31 is connect by hollow tubular structures with feed inlet 21, i.e. feed inlet 21 in example 1 It is passed through raw material from the hollow tubular structures in second supporter 31 to flow-guiding structure 3, raw material can pass through the second supporter 31 Through-hole on tube wall is full of diversion cavity.And if being provided between the second supporter 31 and the first supporter 301 in diversion cavity Evenly spaced floor 32 is done, to further strengthen the structure of flow-guiding structure 3.
Simultaneously in example 1, the aperture that the aperture of the second supporter 31 is greater than the first supporter 301 is greater than filter material 302 Aperture.
In example 1, the working method and principle of reaction kettle are as follows:
First to the first raw material is placed in inside reaction chamber 12, which can be liquid or gas, then pass through institute The feed inlet 21 stated is passed through the second raw material into flow-guiding structure 3, which can be liquid or gas.To which second is former Material can be saturating from the filter opening on several 3 permeable members 30 of flow-guiding structure after being passed into reaction chamber 12 in the flow-guiding structure 3 It crosses and realizes between the first raw material and the second raw material with biggish contact area;The charging to feed inlet 21 can be passed through simultaneously Speed is controlled, thus realize from the second raw material from flow-guiding structure 3 with certain speed and pressure injection to the first raw material, Realization stirs the disperse system in reaction chamber 12 using the second raw material, and then realizes that each phase substance in disperse system is sufficiently mixed It closes.
Secondly, the filter material 302 in flow-guiding structure 3 in embodiment one is also able to achieve the reaction in reaction kettle in disperse system Solid matter in object reactant and/or product and/or catalyst is isolated in the inside or outside of flow-guiding structure 3.As By controlling the hybrid mode of raw material reactant, the solid matter in disperse system is filtered to be realized using filter material 302 Separation.Being separated by filtration described in wherein can be the diversion cavity by the solid matter filtering in disperse system in 3 inside of flow-guiding structure In, it is also possible to filter solid matter in the reaction chamber 12 in 3 outside of flow-guiding structure.
Also, the solid matter in disperse system may be the product after reaction, it is also possible to it is anti-that excessive solid phase be added Object is answered, can also be catalyst.
A kind of more specific three-phase flow catalytic reaction method is provided on the basis of the above embodiments below.Specifically A kind of formaldehyde and acetylene are as raw material reactant, using the copper bismuth catalyst of solid as catalyst, to react generation liquid 1,4- butynediols.
In three flow catalytic reaction methods, first merging has Liquid for maldehyde in the reaction chamber 12 in autoclave body 1, and And acetylene gas, and the reaction chamber 12 on the outside of 3 diversion cavity of flow-guiding structure are passed through into flow-guiding structure 3 by each air inlet 21 In be placed with the copper bismuth catalyst of solid.
In example 1, discharge port 22 is first closed, feed inlet 21 is opened and is passed through acetylene gas, be passed through in embodiment one Control is in 20m/s or more after the velocity-stabilization of acetylene.To which in presently implemented example one, acetylene gas is passed through from 1 bottom position of autoclave body It crosses flow-guiding structure 3 and is passed into reaction chamber 12, since formaldehyde is easy to penetrate into flow-guiding structure 3, so just starting The pressure of bottom position is maximum in flow-guiding structure 3, can thus make substance in flow-guiding structure 3 through filter material 302 to reaction Chamber 12 be discharged, can also be realized in this way by acetylene gas in former reaction chamber 12 Liquid for maldehyde and catalyst stir It is dynamic.
As air inlet 21 is gradually increased to the gas flow that flow-guiding structure 3 is passed through, the pressure in flow-guiding structure 3 gradually increases Greatly, the substance also allowed in flow-guiding structure 3 is gradually increased through filter material 302 to the speed that reaction chamber 12 is discharged, with process The substance speed of filter material 302 reaches a timing, then can make solid particle to the agitation in Liquid for maldehyde by acetylene gas The movement of catalyst aggravates, and gradually solid particle catalyst is held up by gas and suspended state is presented, and realizes that catalyst granules is dividing It dissipates and is fluidized in system.
After catalysis reaction is completed, air inlet 21 is closed, stopping is passed through acetylene gas, is then turned on later positioned at autoclave body The discharge port 22 that 1 bottom end is connect with flow-guiding structure 3 exports the Isosorbide-5-Nitrae of obtained product liquid-butynediols, herein In the process, filter material 302 made of flexible, porous metal foil may be implemented the catalyst of the solid phase in disperse system on flow-guiding structure 3 Filtering is isolated in reaction chamber 12.
Embodiment two includes autoclave body 1 as shown in figure 4, reaction kettle in the present embodiment, and reaction is equipped in the autoclave body 1 Chamber 12 includes the flow-guiding structure 3 of several tubular structures in the reaction chamber 12, which includes above to use Flexible, porous metal foil the permeable member 30 formed on the first supporter 301 is covered in as filter material 302.
Wherein several flow-guiding structures 3 divides for two types, one kind be the first flow-guiding structure 3a be located in reaction chamber 12 and It is connected to feed inlet 21;Another kind is that the second flow-guiding structure 3b is located in reaction chamber 12 and is connected to discharge port 22.By reactant From being passed through in the first flow-guiding structure 3a after reaction chamber 12 reacted, it is discharged from the second flow-guiding structure 3b from discharge port 22.

Claims (5)

1. reaction kettle includes autoclave body (1), reaction chamber (12) are equipped in the autoclave body (1), it is characterised in that: the reaction chamber It (12) include flow-guiding structure (3) in, which includes permeable member (30), and wherein flow-guiding structure (3) is communicated with Feed inlet (21) and discharge port (22), reactant from feed inlet (21) be passed through after by permeable member (30) enter reaction chamber (12) It reacts, obtained product is discharged by the discharge port (22) that permeable member (30) are connected to from flow-guiding structure (3);It is described Flow-guiding structure (3) is tubular structure, and wherein permeable member (30) is located on tube wall;What the permeable member (30) of tubular structure surrounded It include the second supporter of porous hollow tubulose (31) being axially arranged along tube body in diversion cavity, the second supporter (31) week Several evenly spaced floors (32) are equipped between body and permeable member (30) inner wall;Autoclave body (1) lower end is set close to lower end There are feed inlet (21) and discharge port (22), middle charging aperture (21) and discharge port (22) are two same flow-guiding structures of parallel branch (3) it is connected to, the lower end of second supporter (31) is connected to the feed inlet (21), the permeable member (30) and the second support The lower end of diversion cavity between body (31) is connected to discharge port (22).
2. reaction kettle as described in claim 1, it is characterised in that: the permeable member (30) includes table body aperture first Support body (301), the permeable member (30) further include having the filter material (302) to fit with first supporter (301).
3. reaction kettle as claimed in claim 2, it is characterised in that: the permeable member (30) is located at filter material (302) and sets on one side There is compressing member;The filter material (302) uses a kind of flexible, porous metal foil.
4. reaction kettle as described in claim 1, it is characterised in that: several flow-guiding structures (3) are equipped in the autoclave body (1), Middle flow-guiding structure (3) is located in reaction chamber (12) to be fixedly connected with autoclave body (1) upper and lower side respectively, and wherein autoclave body (1) is equipped with several Mutually independent feed inlet (21) and discharge port (22) are connect with each flow-guiding structure (3) respectively.
5. the three-phase flow catalytic reaction method of reaction kettle described in any one of application Claims 1 to 4, it is characterised in that: described Reaction kettle includes for containing the reaction chamber of material liquid (12), and reaction kettle includes the feed inlet for being passed through unstripped gas (21) discharge port (22) and for liquid product to be discharged;Material liquid is placed in reaction chamber (12) first, by solid catalysis Agent is placed in reaction chamber (12), unstripped gas is passed through in reaction chamber (12) from feed inlet (21), to close charging after the reaction was completed Mouth (21) opens discharge port (22) and exports liquid product.
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