CN105080446B - A kind of multistage charging hypergravity L-L reactor device and its application - Google Patents
A kind of multistage charging hypergravity L-L reactor device and its application Download PDFInfo
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Abstract
The invention discloses a kind of multistage charging hypergravity L-L reactor device, including rotor, case top lid, liquid distribution trough and housing；The housing lower end is provided with liquid outlet；It is characterized in that：The liquid distribution trough includes interior liquid distribution trough and outer liquid distribution trough；The rotor provided with the different concentric insertion ring of diameter, and it is built-in in the housing；Communicated between the insertion ring and case top lid provided with the space between space, and the concentric insertion ring and case top lid of different-diameter；The interior liquid distribution trough is extended in the middle part of rotor；The outer liquid distribution trough is extended respectively into the space between concentric insertion ring.Without sealing device between the insertion ring top of apparatus of the present invention and case top lid；The liquid distribution trough of device can realize multistage charging in internal rotor；The rapidly and uniformly molecular scale mixing needed for parallel reaction and consecutive reaction can be realized, so as to be remarkably improved reaction selectivity, with the outstanding advantages such as accessory substance is few, product yield is high.
Description
Technical field
The present invention relates to a kind of multistage charging hypergravity L-L reactor device and its application.The device can be applied to fast
The reactive liquid solution systems such as the parallel, consecutive of speed, belong to supergravity technical field.
Background technology
Chemical reaction is the process that atom is rearranged, even single reactant, feelings are rearranged due to atom
Condition is different, and the product of generation is also varied.Parallel reaction and consecutive reaction are two kinds of common reaction systems.It is general and
Speech, its reaction species number is generally higher than equal to 2.For parallel reaction, reactant can abreast carry out two or two simultaneously
Differential responses more than individual, draw different products.The reaction referred to as main reaction of desired product can be wherein generated, remaining is referred to as pair
Reaction.Its reaction equation can use following formula to express（R represents desired product, and S represents accessory substance, and A and B represent reactant）：
A+B → R or A+B → R
A+B→SA+A→S
Such as the nitration reaction of phenol, ortho position, contraposition, three kinds of nitrophenols of meta can be obtained, principal product is o-nitrophenol（About
Account for 59%）；Ethanol can abreast carry out two kinds of reactions of dehydration and dehydrogenation..The ratio between product amount of each reaction of parallel reaction is equal to
The ratio between its reaction rate constant.The selectivity of some parallel reactions can be changed by changing reaction temperature or addition special catalyst etc..
For quick parallel reaction, shorten the time of microcosmic mixing between reactant, and make a kind of reactant therein significantly excessive,
The selectivity of desired product can be greatly improved.
For consecutive reaction, its reaction equation can use following formula to express：
A+B → R or A+B → R
B+R→SA+R→S
If A can be well mixed rapidly with B, rapid reaction exhausts and stopped, then is generated without S；If instead generating S,
Illustrate there must be component to be separated, A and B mixing are uneven, there is bad haptoreaction.Such as methanol and ammonia reaction, charge ratio is not
It is same to generate methylamine, dimethylamine, trimethylamine.Reaction is as follows：
For above two reaction, its selectivity how is improved, the yield for improving product is the core of reaction engineering research
Heart problem.For quickly parallel and consecutive reaction system, feed way, incorporation time and the relation in reaction time, reactant
Mol ratio etc. the process of reaction can all have been influenceed.Conventional stirred tank is done because blade is fixed on certain point to liquid
Work(, is only locally realizing mixing, it is impossible to which the molecular level needed for uniformly realizing fast and parallel reaction and consecutive reaction is other microcosmic mixed
Close.Although in industrial operation, reactant A is added drop-wise into reactant B（Assuming that B is significantly excessive）In, make reactant A as far as possible
Quickly consume.But by stirred tank it is intrinsic it is hydromechanical influence, cause that the selectivity of its product is low, accessory substance is more.In work
In the application of industry scale, for the fast and parallel or consecutive reaction that heat release is violent, stirred tank is designed as multi-floating bodies by designer
Or cascade reactor, reactant A is evenly spread in each reactor, makes every effort to reactant A being dispersed in reactor
In.But multi-floating bodies or cascade reactor there are problems that bulky, flow it is complicated,.
The content of the invention
The invention solves the problems that first technical problem be to provide a kind of multistage charging hypergravity L-L reactor device.Should
The rotor of device is made up of the different packing ring of diameter, and it is built-in in the housing.Rotor endcap is filled with case top lid without sealing
Put.The liquid distribution trough of device can realize multistage charging in internal rotor.It is apparatus of the present invention small volume, simple and compact for structure；Can
To realize the microcosmic mixing of the molecular scale needed for uniform fast and parallel reaction and consecutive reaction, so as to reduce the production of accessory substance
It is raw, improve product yield.
The invention solves the problems that second technical problem be to provide said apparatus in reactive liquid solutions such as quick parallel, consecutives
Application in system.
To solve above-mentioned first technical problem, the invention provides a kind of multistage charging hypergravity L-L reactor dress
Put, including rotor, case top lid, liquid distribution trough and housing；The housing lower end is provided with liquid outlet；The liquid distribution trough
Including interior liquid distribution trough and outer liquid distribution trough；
The rotor provided with the different concentric insertion ring of diameter, and it is built-in in the housing；
Be provided with space between the insertion ring and case top lid, and different-diameter concentric insertion ring and case top lid it
Between space communicate, that is, without sealing device between each insertion ring top and case top lid；
The interior liquid distribution trough is extended in the middle part of rotor, and liquid can be sprayed from inside to outside；
The outer liquid distribution trough is extended respectively into the space between concentric insertion ring, can from inside to outside or from
Liquid is sprayed outside to inside so that outer liquid distribution trough can realize multistage charging in internal rotor.
Preferably, the insertion ring is filled out selected from stainless steel cloth filler, random packing, nano-micro structure filler, microchannel
Material, monoblock type silicon carbide filler, metal foam filler or the solid packing with catalysis.
Preferably, the number of turns of the concentric insertion ring is enclosed for 2-10；It is highly preferred that the number of turns of the concentric insertion ring
Enclosed for 3-6.
Preferably, the reactant of described reactive liquid solution is more than or equal to 2 kinds liquid.
Preferably, the reactant of described reactive liquid solution can add catalyst, and catalyst can be liquid or solid.It is preferred that
Ground, in single rotary shaft, it is 1-5 that the rotor of built-in multi-turn insertion ring, which installs number,.It is highly preferred that number is 1-3.
Preferably, rotary shaft mounting means may be either horizontal, or vertical.
To solve above-mentioned second technical problem, device as described above should the reaction systems such as quick parallel, consecutive
With；Rotor speed 10-4000rpm；- 30-300 DEG C of operation temperature in reaction cavity；The preferred 0.01- of operating pressure in reaction cavity
50MPa；It is highly preferred that rotor speed 250-2500rpm；- 5-200 DEG C of operation temperature in reaction cavity；Reaction chamber in-vivo procedures
The preferred 0.1-10MPa of pressure；Most preferably, rotor speed 400-1500rpm；0-150 DEG C of operation temperature in reaction cavity；Reaction
The preferred 0.1-5MPa of operating pressure in cavity.
Preferably, described quick reactive liquid solution system, its intrinsic reaction half-time is less than 100 second-times；It is preferably small
In 10 second-times；More preferably less than 1 second-time.
Preferably, quick reactive liquid solution system is condensation, rearrangement, azo, sulfonation, alkylation, nitrification, halogenation, polymerization
Or reactive crystallization system.
The present invention has the advantages that：
The rotor of apparatus of the present invention is made up of the different packing ring of diameter, and it is built-in in the housing；Rotor endcap and housing
Upper lid is without sealing device；The liquid distribution trough of device can realize multistage charging in internal rotor；Apparatus of the present invention small volume, knot
Structure is simply compact；It can realize the microcosmic mixing of the molecular scale needed for uniform fast and parallel reaction and consecutive reaction, and can be
Reactor along along journey according to needed for intrinsic reaction, neatly modulation reactant molar ratio, so that in the reaction microcell of molecular scale
Ideal response environment required when intrinsic reaction is carried out with high selectivity is inside realized, so as to substantially reduce the generation of accessory substance, is carried
High product yield, reduces material consumption and the energy consumption of unit product.
Brief description of the drawings
Fig. 1 is a kind of structural representation of multistage charging hypergravity L-L reactor device of the present invention；
Fig. 2 is the reaction unit of the present invention in quick parallel, consecutive reaction system application flow schematic diagram.
Embodiment
Embodiment of the present invention is described further with reference to the accompanying drawings and examples.But the invention is not restricted to listed
The embodiment gone out.
Embodiment 1
It is shown in Figure 1, a kind of multistage charging hypergravity L-L reactor device 100, including rotor 101, case top lid
102nd, liquid distribution trough 103 and housing 104；The lower end of housing 104 is provided with liquid outlet 105；The liquid distribution trough 103 is wrapped
Include interior liquid distribution trough 1031 and outer liquid distribution trough 1032；
The rotor 101 is built in housing 104 provided with the different concentric insertion ring 106 of diameter；
Space 107, and the concentric insertion ring 106 of different-diameter are provided between the insertion ring 106 and case top lid 102
Space between case top lid 102 is communicated, that is, need not between the top of each insertion ring 106 and case top lid 102
Sealing device；
The interior liquid distribution trough 1031 extends to the middle part of rotor 101, and liquid can be sprayed from inside to outside；
The outer liquid distribution trough 1032 is extended respectively into the space 108 between concentric insertion ring 106, can be in
Spray outwards or from the outside to the core liquid.So that multistage charging can be achieved in outer liquid distribution trough 1032 inside rotor 101.
Further improved embodiment, the insertion ring is filled out selected from stainless steel cloth filler, random packing, nano-micro structure
Material, microchannel filler, monoblock type silicon carbide filler, metal foam filler or the solid packing with catalysis.
Further improved embodiment, the number of turns of the concentric insertion ring is enclosed for 2-10；It is highly preferred that described concentric
The number of turns of insertion ring is enclosed for 3-6.In the present embodiment shown in the drawings of 4 circles.
Further improved embodiment, in single rotary shaft, it is 1-5 that the rotor of built-in multi-turn insertion ring, which installs number,
It is individual；It is highly preferred that number is 1-3；1 is shown in the present embodiment.
Further improved embodiment, rotor mounting means may be either horizontal, or vertical.Show in the present embodiment
It is vertical.
Embodiment 2
It is shown in Figure 2, to include the reactive liquid solution system dress of multistage charging hypergravity L-L reactor device of the invention
Put, wherein, the first head tank 201 is arrived by pipeline communication to the first feed pump 202, first feed pump by pipeline communication
Outer liquid distribution trough 1032；Second head tank 301 is passed through by pipeline communication to the second feed pump 302, second feed pump
Pipeline communication is to interior liquid distribution trough 1031；The connection outlet pipeline 1051 of liquid outlet 105 of the lower end of housing 104；Second
Head tank 301 is connected with outlet conduit 1051 by pipeline and communicated.
Embodiment 3
It is shown in Figure 2, include the reactive liquid solution system and device of multistage charging hypergravity L-L reactor device of the invention
Application in Beckmann rearrangement, is comprised the following steps that：
1）Raw material cyclohexanone oxime and cryogen heptane are pumped into multistage charging hypergravity liquid liquid of the invention through the first feed pump
The outer liquid distribution trough 1032 of reactor assembly；Design parameter is：The volume ratio of cyclohexanone oxime and cryogen heptane is 1:13, altogether
18L；
2）Raw material amidatioon liquid is pumped into multistage charging hypergravity L-L reactor device of the invention through the second feed pump
Interior liquid distribution trough 1031；Design parameter is：The volume ratio for the mixed liquor that amidatioon liquid and the first feed pump are pumped into is 0.9:
1；
3）Regulation rotor speed is that operation temperature and pressure are 90 DEG C, 0.3MPa in 2000r/min, reaction cavity；Reaction
Product afterwards is discharged from liquid outlet 105.Through analysis, the conversion ratio of cyclohexanone oxime is 100%, and the selectivity of caprolactam is
99.9%。
Comparative example 1：
Embodiment 3 is repeated, its difference is, react and carried out in conventional supergravity reactor, raw material cyclohexanone
Oxime and cryogen heptane are all contacted in the first order of the outer liquid distribution trough shown in Fig. 2 with from interior liquid distribution trough amidatioon liquid
And react, reacted product is discharged from liquid outlet 105, and the conversion ratio of cyclohexanone oxime is 98%, the selection of caprolactam
Property is 92.7%.
Embodiment 4
It is shown in Figure 2, include the reactive liquid solution system and device of multistage charging hypergravity L-L reactor device of the invention
Application in alkylated reaction, is comprised the following steps that：
1）Raw material C 4 mixture is pumped into multistage charging hypergravity L-L reactor of the invention through the first feed pump to fill
The outer liquid distribution trough 1032 put；Design parameter is：The mol ratio of iso-butane and isobutene is 10:1；
2）Raw material containing ionic-liquid catalyst is pumped into multistage charging hypergravity liquid liquid of the invention through the second feed pump
The interior liquid distribution trough 1031 of reactor assembly；
3）Regulation rotating speed is 1500r/min, in reaction cavity operation temperature and pressure be 0.4MPa, 6 DEG C.Reacted production
Thing is discharged from liquid outlet 105, after testing, and the octane number of reaction product is 98.
Comparative example 2：
Embodiment 4 is repeated, its difference is, react and carried out in conventional supergravity reactor, material carbon four is mixed
Compound the outer liquid distribution trough shown in Fig. 2 the first order all with from interior liquid distribution trough containing ionic-liquid catalyst
Raw material is contacted and reacted, and reacted product is discharged from liquid outlet 105, and the octane number of reaction product is 92.
Embodiment 5
It is shown in Figure 2, include the reactive liquid solution system and device of multistage charging hypergravity L-L reactor device of the invention
Application in nitrification parallel reaction, is comprised the following steps that：
1）Raw material 2,4- dinitrophenol is pumped into multistage charging hypergravity reactive liquid solution of the invention through the second feed pump
The interior liquid distribution trough 1031 of device device；Design parameter is：2,4- dinitrophenol quality is 0.5Kg.
2）The mixture of raw material dichloromethane and water is pumped into multistage charging hypergravity liquid of the invention through the first feed pump
The outer liquid phase distributor of the outer liquid distribution trough 1032 of liquid reactor assembly；Design parameter is：The volume ratio of dichloromethane and water
For 1.5:1.
3）It is 20 DEG C, 0.1Mpa to adjust operation temperature and pressure in rotating speed 1000rpm, reaction cavity.Again to reaction cavity
Inside it is slowly injected into 0.0275L65% nitric acid.Reacted product is discharged from liquid outlet 105, after testing, reaction product yield
For 92%.
Comparative example 3：
Embodiment 5 is repeated, its difference is, react and carried out in conventional supergravity reactor, its reaction product
Yield be generally 64-77%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (16)
1. a kind of multistage charging hypergravity L-L reactor device, including rotor, case top lid, liquid distribution trough and housing；Institute
Housing lower end is stated provided with liquid outlet；It is characterized in that：The liquid distribution trough includes interior liquid distribution trough and outer liquid distribution
Device；
The rotor provided with the different concentric insertion ring of diameter, and it is built-in in the housing；
It is provided between the insertion ring and case top lid between space, and the concentric insertion ring and case top lid of different-diameter
Space is communicated；
The interior liquid distribution trough is extended in the middle part of rotor；
The outer liquid distribution trough is extended respectively into the space between concentric insertion ring.
2. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：The insertion ring choosing
From stainless steel cloth filler, random packing, nano-micro structure filler, microchannel filler, monoblock type silicon carbide filler, foam metal
Filler or the solid packing with catalysis.
3. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：Described concentric fills out
The number of turns of feed ring is enclosed for 2-10.
4. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：Described concentric fills out
The number of turns of feed ring is enclosed for 3-6.
5. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：Described liquid liquid is anti-
The reaction mass answered is more than or equal to 2 kinds liquid, and the liquid realizes that reaction moves the liquid of heat comprising phase transformation.
6. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：Described liquid liquid is anti-
The reactant answered adds catalyst, and catalyst is liquid or solid slurry.
7. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：In single rotary shaft
On, it is 1-5 that the rotor of built-in multi-turn insertion ring, which installs number,.
8. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：In single rotary shaft
On, it is 1-3 that the rotor of built-in multi-turn insertion ring, which installs number,.
9. multistage charging hypergravity L-L reactor device according to claim 1, it is characterised in that：Rotor mounting means
To be horizontal or be vertical.
10. any device is in quick parallel, consecutive, parallel-consecutive complex reaction system in claim 1-9 as described above
Using；It is characterized in that：Rotor speed 10-4000 rpm；- 30-300 DEG C of operation temperature in reaction cavity；Grasped in reaction cavity
Make pressure 0.01-50 MPa.
11. any device is in quick parallel, consecutive, parallel-consecutive complex reaction system in claim 1-9 as described above
Using；It is characterized in that：Rotor speed 250-2500 rpm；- 5-200 DEG C of operation temperature in reaction cavity；Grasped in reaction cavity
Make pressure 0.1-10 MPa.
12. any device is in quick parallel, consecutive, parallel-consecutive complex reaction system in claim 1-9 as described above
Using；It is characterized in that：Rotor speed 400-1500 rpm；0-150 DEG C of operation temperature in reaction cavity；Reaction chamber in-vivo procedures
Pressure 0.1-5 MPa.
13. according to any described applications of claim 10-12；It is characterized in that：Described quick parallel, consecutive, it is parallel-
Consecutive complex reaction system, its intrinsic reaction half-time is less than 100 second-times.
14. according to any described applications of claim 10-12；It is characterized in that：Described quick parallel, consecutive, it is parallel-
Consecutive complex reaction system, its intrinsic reaction half-time is less than 10 second-times.
15. according to any described applications of claim 10-12；It is characterized in that：Described quick parallel, consecutive, it is parallel-
Consecutive complex reaction system, its intrinsic reaction half-time is less than 1 second-time.
16. according to any described applications of claim 10-12；It is characterized in that：Quick parallel, consecutive, parallel-consecutive are multiple
Miscellaneous reaction system is condensation, rearrangement, azo, sulfonation, alkylation, nitrification, halogenation, polymerization or reactive crystallization system.
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| CN106397081A (en) * | 2015-07-14 | 2017-02-15 | 北京化工大学苏州（相城）研究院 | Halogenation reaction method |
| CN106430119A (en) * | 2016-08-30 | 2017-02-22 | Tcl集团股份有限公司 | Quantum dot synthesis amplification method |
| CN110882663B (en) * | 2018-09-10 | 2021-07-27 | 临沂大学 | Hypergravity micro-reaction device |
| CN109569346B (en) * | 2019-01-22 | 2020-09-15 | 北京化工大学 | High-energy-efficiency dispersing-mixing method for large-phase-ratio system and application thereof |
| CN111659311B (en) * | 2020-06-05 | 2021-05-14 | 北京化工大学 | Method for enhancing mixing performance of rotating packed bed based on liquid distributor with super-hydrophobic surface |
| CN113387858A (en) * | 2021-06-29 | 2021-09-14 | 山东尚舜化工有限公司 | Equipment and method for continuously producing accelerant TMTD |
| CN116139788A (en) * | 2023-03-10 | 2023-05-23 | 北京化工大学 | Device, system and method for continuously producing cyclohexanone oxime |
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Effective date of registration: 20220126 Address after: 324000 No. 5, Wenjiao West Road, Shuangta street, Jiangshan City, Quzhou City, Zhejiang Province Patentee after: Zhejiang zhongjuhairui Technology Co.,Ltd. Address before: 100029, No. 15 East Third Ring Road, Chaoyang District, Beijing Patentee before: BEIJING University OF CHEMICAL TECHNOLOGY |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170815 |