CN104368301A - Hyper-gravity reactor and reaction method - Google Patents
Hyper-gravity reactor and reaction method Download PDFInfo
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- CN104368301A CN104368301A CN201310352689.XA CN201310352689A CN104368301A CN 104368301 A CN104368301 A CN 104368301A CN 201310352689 A CN201310352689 A CN 201310352689A CN 104368301 A CN104368301 A CN 104368301A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/03—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of non-aromatic carbon-to-carbon double bonds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a hyper-gravity reactor and a reaction method. The hyper-gravity reactor is provided with two liquid inlets. Two liquid inlets are respectively connected to responding liquid distributors. The spraying pipes of two liquid distributors are separated and arranged on concentric rings, which take the middle shaft of a rotation bed as the center. The reaction method comprises the following steps: feeding a reaction material and a catalyst or two reaction materials into the hyper-gravity reactor from the two liquid inlets, then spraying the reaction material and the catalyst or two reaction materials on the internal edges of rotating filling materials or solid catalysts from two individual spraying pipes so as to mix the reaction material and the catalyst or two reaction materials, carrying out reactions by contacting the reaction material and the catalyst or two reaction materials, or carrying out reactions by contacting the mixture with gas. The structure and distribution of the liquid inlets and spraying pipes of the hyper-gravity reactor are both improved so as to mix the liquid catalyst and liquid reactant in a hyper-gravity field, because the mixing effect is good in a hyper-gravity field. At the same time the problems of the post treatment for separating the liquid catalyst and the liquid products are also solved and simplified.
Description
Technical field
The present invention relates to reaction engineering field, furtherly, relate to a kind of supergravity reactor and reaction method.
Background technology
Catalytic reaction is in petrochemical industry; the field such as chemical industry, bioengineering, environmental protection is ubiquitous; catalytic reaction is carried out in all kinds of reactor such as such as fixed bed, fluid bed etc.; the physical space that reactor provides reaction mass, reaction mass and homogeneous phase or heterogeneous catalyst to come in contact; the type selecting of reactor often determines reaction mass; the way of contact of reaction mass and catalyst, most important on the impact of catalytic reaction efficiency.
High-gravity technology is the engineering that twentieth century grows up the seventies, and the EP0023745A3 patent of ICI Imperial Chemical Industries of Britain (ICI) relates to chemical separating unit operations---the research of the processes such as-distillation, absorption, desorb.
Chinese patent CN1507940A discloses the method for carrying out catalytic reaction in super gravity field, the method adopts high-gravity rotating bed as catalytic reactor, catalyst is fixed on revolving bed rotor, involved catalytic reaction is homogeneous phase or heterogeneous reaction, the method can reduce accessory substance and generate, reduce equipment volume, reduce energy consumption.
Chinese patent CN1743064A discloses a kind of by after heterogeneous catalyst liquid phase, carries out the method for catalytic reaction in high-gravity rotating bed.Wherein said liquid phase refers to and catalyst activity components dissolved is formed homogeneous mixture in liquid phase reactor thing or solvent, or it is dispersed in liquid phase reactor thing or solvent with fine particle.The method extends the regeneration period of catalyst, improves production efficiency.
Chinese patent CN1895766A discloses a kind of process for selective hydrogenation, deimpurity for hydrocarbon material selec-tive hydrogenation process is carried out by the method in rotating bed super gravity, selective hydrocatalyst is fixed on revolving bed rotor, the method adjusts the time of staying of hydrocarbon material at beds by regulating high-gravity rotating bed rotor speed and rotor radial thickness, thus controlling the selective of hydrogenation, the method is different from traditional selec-tive hydrogenation technique.
But all there is following point in above patent: if between multiply liquid material during intersolubility difference, there is local mixing inequality or solution lamination in mixed solution, then when this mixture flow to into super gravity field to contact with beds react time, obvious reaction is also only present in the local of beds, have considerable part between different liquid materials cannot contact with each other each other, reaction conversion ratio can not be desirable.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of supergravity reactor and reaction method.Present invention improves over structure and the layout of supergravity reactor liquid inlet opening and shower, liquid catalyst and liquid reactant or being blended in super gravity field of two kinds of liquid reactions materials are carried out, gives full play to the advantage of good mixing effect in Elevated Gravity; Solve simultaneously and simplify the problem of later separation.
An object of the present invention is to provide a kind of supergravity reactor.
Described supergravity reactor is provided with two liquid inlet openings, and two liquid inlet openings connect respective liquid distribution trough respectively, and the shower of two liquid distribution troughs is independent separately and be arranged at on the revolving bed axis donut that is the center of circle.
Preferred:
The shower number of described two liquid distribution troughs is identical and be spaced successively.
Two of object of the present invention is to provide a kind of reaction method adopting described supergravity reactor.
Comprise:
Reaction mass and catalyst or two kinds of reaction masses enter supergravity reactor from two liquid inlet openings respectively, and be sprayed on rotation filler or solid catalyst inner edge via respective shower, both realizations mix, contact simultaneously reacts, or rear the contact with gas phase of mixing reacts.
Reacted liquid-phase product and catalyst enter Liquid level tank by supergravity reactor liquid-phase outlet, then enter separation of products tank, and product material is separated by static layering with liquid catalyst.
A catalyst part after separation goes regeneration process, and another part is for recycling.
For the reaction of two bursts of liquid materials, when reacting generation precipitation, if intersolubility is poor between liquid material, then can realize liquid-liquid-solid separation by natural layering: if simultaneously when this reaction is catalytic reaction, if now catalyst liquid phase form, then catalyst is by dissolving each other with wherein a certain liquid material and realize being separated with another kind of liquid material; If catalyst solid granular form fills in packed bed, then the liquid layered only related between reaction liquid material is separated.Liquid material situation after visual response and determining, two bursts of liquid materials can utilize or recycle use after treatment by direct circulation.
For gas-liquid catalytic reaction process, course of reaction of the present invention is illustrated below:
Liquid reaction material and liquid catalyst enter supergravity reactor by each self-corresponding liquid inlet, and be sprayed on rotation filler inner edge via respective shower, mixing both realizing in filler, contacts with gas phase simultaneously and catalytic reaction (the full hydrogenation of such as carbon four or selective hydrogenation process) occurs.Reacted liquid-phase product and catalyst enter Liquid level tank by supergravity reactor liquid-phase outlet, then enter separation of products tank, and product material is separated by static layering with liquid catalyst.A catalyst part after separation goes regeneration process, and another part is for recycling, and product material enters follow-up flow process deep processing process.
Liquid reaction material and liquid catalyst separate feeds separately in the present invention, enter respective liquid distribution trough, the shower of the two is positioned on annulus (with revolving bed axis for annulus) independent but concentric separately, here two cover distributors shower number is separately to be all the best mutually, and be spaced successively, to reaching best mixed effect.
The present invention is significant for the practical application in industry of liquid-phase catalyst, this is because an importance of limits liquid phase catalyst practical application is exactly the later separation problem needing to consider liquid reaction product and liquid-phase catalyst.Simple consideration product separation, wish liquid reaction/product and liquid catalyst intersolubility poor, make simple process can complete reactant, product is separated with catalyst, but traditional reactor material contact feature determines such liquid reaction/product and catalyst combination must exist the problem that mass transfer effect is not good, reaction conversion ratio is low, affects reaction efficiency; Therefore simple from reaction angle consider wish that liquid reactant and catalyst have good intersolubility, both liftings contact area, to promote mass transfer.Condition each other with reaction two aspect factors owing to being separated, directly limit the application of liquid-phase catalyst, all benefits that it is had only rest on theoretic, cannot put into practice.The catalysis process that patent CN1743064A proposes is intended to strengthen mass transfer, but it is good and do not need or the operating mode of less consideration later separation problem that its liquid reaction material and catalyst are only applicable to the two intersolubility in super gravity field [centrifugal acceleration that the filling batch (or beds) that super gravity field refers to rotation produces is greater than the centrifugal force field of acceleration of gravity G] outer premix pattern, and this obviously limits the industrial applicability of liquid-phase catalyst.In super gravity field, both realized liquid reaction material in the present invention mix with the degree of depth of liquid catalyst, also realize alternate mass transfer to maximize simultaneously, breach reaction and the situation being separated two aspects and conditioning each other, for the extensive use of liquid catalyst is opened up the game, make still can fully contact under intersolubility poor condition between liquid catalyst with liquid material, complete reaction, be convenient to later separation again simultaneously.
Especially for catalytic liquid and reactant liquor do not dissolve each other operating mode (or the two dissolve each other but both needing to control time of contact operating mode), advantage of the present invention is particularly evident-react efficiently and mixed liquor is easy to later separation.
Mixing in the present invention in super gravity field and reaction pattern are not limited only to the form of liquid reaction material+liquid catalyst, equally also be applicable to the mixing of multiply liquid reaction material in super gravity field react with (catalysis or on-catalytic), if the words of reaction catalytic process, now catalyst can be fixed on revolving bed in solid form, also can be dissolved in liquid form in (or molecule form is suspended in) a certain liquid reaction material.Namely catalyst can exist by solid granular form, also can adopt liquid phase form, wherein preferred liquid phase form; Present invention improves over the hybrid mode of catalyst and liquid phase reacting material, make catalyst and mixing between liquid phase reactor thing and vapor-phase reactant more abundant, avoid in CN1743064A the reaction mass that adopts the outer premix of super gravity field to exist and the uneven problem of catalyst local mixing (when liquid catalyst and liquid phase reactor thing intersolubility is poor or catalytic liquid with particle suspend exist time the most outstanding); Correspondingly present invention improves over structure and the layout of supergravity reactor liquid inlet opening and shower, liquid catalyst and being blended in super gravity field of liquid reactant are carried out, gives full play to the advantage of good mixing effect in Elevated Gravity; The present invention simultaneously solves and simplifies the problem of liquid catalyst and liquid product later separation.
The present invention requires low to the intersolubility between multiply liquid material, and this has just widened the scope of application of high-gravity technology for catalysis/on-catalytic field greatly, also solves the thorny problem of material later separation.
Accompanying drawing explanation
Fig. 1 supergravity reactor structural representation of the present invention
The front view of the shower of Fig. 2 liquid distribution trough
The upward view of the shower of Fig. 3 liquid distribution trough
Fig. 4 the present invention is used for the schematic flow sheet of catalytic hydrogenation reaction
Description of reference numerals:
1 liquid inlet opening; 2 gas accesses; 3 fillers; 4 rotors; 5 showers; 6 liquid outlets; 7 gas vents; 8 liquid spouts; 9 head tanks; 10 catalyst storage tanks; 11 supergravity reactors; 12 Liquid level tanks; 13 separation of products tanks; 14 hydrogenated products; 15 catalytic liquid go regeneration; 16-hydrogen; 17-hydrogenation tail gas
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment:
As shown in Fig. 1, Fig. 2, Fig. 3, a kind of supergravity reactor.Described supergravity reactor 11 is provided with two liquid inlet openings 1, two liquid inlet openings 1 connect respective liquid distribution trough respectively, the shower 5 of two liquid distribution troughs is independent separately and be arranged at on the revolving bed axis donut that is the center of circle, and the shower number of described two liquid distribution troughs is identical and be spaced successively.
Catalyst preparing: this catalyst uses nitric acid and hydrochloric acid 1:1 proportioning concentration to be dissolved by metal Pd, control the Pd particle size after dissolving within the scope of 5-50nm, then use NaOH solution to regulate solution Ph value between 6.5-7, finally add deionized water and make aqueous phase catalyst.Active component Pd with nano particle state even suspension (similar dissolving), should be noted in preparation process that control nano level active component Pd does not precipitate and does not assemble in whole solution.
Supergravity reactor as shown in Figure 1, flow process as shown in Figure 4, hydrogen tangentially enters reactor by gas access, liquid-phase C four raw material and liquid-phase catalyst enter respective liquid distribution trough by respective liquid inlet respectively, and be sprayed on rotation filler inner edge through respective shower, in filler, realize the mixing of liquid, simultaneously with hydrogen counter current contacting, hydrogenation reaction occurs.
Reaction condition: inlet temperature 25 DEG C, pressure 25atm, air speed 60hr
-1, hydrogen/unsaturated bond 1.0mol/mol, filler is woven wire, and porosity is 98.5%, supergravity reactor rotating speed 1800rmin
-1.
After reaction, gas from gas outlet is derived; After reaction, liquid mixture imports Liquid level tank by liquid outlet, and then enter control of product tank, carbon four oil phase product and aqueous phase catalyst realize natural separation.
The full hydrogenated products of carbon four remove following process unit; Depending on liquid-phase catalyst performance, a part can enter catalytic liquid storage tank for circulation hydrogenation, a part goes the regeneration of regeneration process workshop section.
Comparative example:
With the full hydrogenation embodiment of C-4-fraction disclosed in Chinese patent CN1743064A as a comparison case.
For effect of the present invention is described, the raw material composition, operating temperature, pressure, the air speed that use in embodiment, supergravity reactor rotor size and rotating speed are all identical with illustrative example in patent CN1743064A, so that compare and illustrate.
The full hydrogenation effect of embodiment and comparative example is in table 1.
Table 1
As can be seen from the table, the full hydrogenation effect in the present embodiment is suitable with comparative example effect, illustrates that liquid catalyst contacts with C 4 materials fully, good mixing effect when the mixed mode adopted in the present invention and shower design, analysis data find, the present invention is when circulating smaller (4 and 3), also full hydrogenation effect is preferably had, this is because liquid catalyst not only plays catalytic action in the reactor, also play cooling effect simultaneously, take away partial reaction heat, and specific heat of water holds apparently higher than carbon four recycle stock, cooling effect is more obvious, this means: adopt the inventive method, C 4 materials recycle ratio can be reduced, that is, reactor load can be reduced under equal production (product) scale, the same materials disposal ability lower unit interval can the more full hydrogenated products of output, good economy performance, simultaneously in the present invention, liquid catalyst is easy to raw material and product to be separated, reduces separation phase and to produce and manpower is born.
Claims (5)
1. a supergravity reactor, is characterized in that:
Described supergravity reactor is provided with two liquid inlet openings, and two liquid inlet openings connect respective liquid distribution trough respectively, and the shower of two liquid distribution troughs is independent separately and be arranged at on the revolving bed axis donut that is the center of circle.
2. supergravity reactor as claimed in claim 1, is characterized in that:
The shower number of described two liquid distribution troughs is identical and be spaced successively.
3. adopt a reaction method for supergravity reactor as claimed in claim 1 or 2, it is characterized in that described method comprises:
Reaction mass and catalyst or two kinds of reaction masses enter supergravity reactor from two liquid inlet openings respectively, and be sprayed on rotation filler or solid catalyst inner edge via respective shower, both realizations mix, contact simultaneously reacts, or rear the contact with gas phase of mixing reacts.
4. reaction method as claimed in claim 3, is characterized in that:
Reacted liquid-phase product and catalyst enter Liquid level tank by supergravity reactor liquid-phase outlet, then enter separation of products tank, and product material is separated by static layering with liquid catalyst.
5. reaction method as claimed in claim 4, is characterized in that:
A catalyst part after separation goes regeneration process, and another part is for recycling.
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| CN201310352689.XA CN104368301B (en) | 2013-08-14 | 2013-08-14 | A kind of supergravity reactor and reaction method |
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| CN201310352689.XA CN104368301B (en) | 2013-08-14 | 2013-08-14 | A kind of supergravity reactor and reaction method |
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| CN104368301B CN104368301B (en) | 2016-08-17 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430108A (en) * | 2016-10-10 | 2017-02-22 | 中国石油大学(北京) | System and method for preparing hydrogen peroxide through anthraquinone method under supergravity condition |
| CN107098824A (en) * | 2017-05-24 | 2017-08-29 | 河南心连心化肥有限公司 | The device and production method of a kind of utilization supergravity reactor production oxamides |
| CN107141251A (en) * | 2017-03-17 | 2017-09-08 | 江苏中邦制药有限公司 | A kind of method for directly synthesizing nanometer small particle ZPT |
| CN107758672A (en) * | 2017-12-04 | 2018-03-06 | 中国恩菲工程技术有限公司 | The recovery method of silica flour in crystalline silicon cutting waste material |
| CN109053412A (en) * | 2018-08-13 | 2018-12-21 | 南京塔川化工设备有限公司 | Homogeneous premixing method before a kind of PTA energy saving device and CTA oxidation reaction |
| CN109647315A (en) * | 2019-01-08 | 2019-04-19 | 北京化工大学 | Super-gravity device, method for oxidation and the system that energy makes full use of |
| CN110903179A (en) * | 2018-09-17 | 2020-03-24 | 中国石油化工股份有限公司 | Method for synthesizing acetone condensation compound by acetone and hydrogen |
| CN111082042A (en) * | 2018-10-21 | 2020-04-28 | 圣戈莱（北京）科技有限公司 | Ternary positive electrode material micron single crystal structure for lithium ion battery and preparation method thereof |
| CN111653796A (en) * | 2020-06-12 | 2020-09-11 | 清华大学 | Batch preparation method of uniform catalyst |
| CN114478614A (en) * | 2022-03-11 | 2022-05-13 | 新疆晶硕新材料有限公司 | Process and apparatus for the preparation of vinylchlorosilanes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106430108A (en) * | 2016-10-10 | 2017-02-22 | 中国石油大学(北京) | System and method for preparing hydrogen peroxide through anthraquinone method under supergravity condition |
| CN107141251A (en) * | 2017-03-17 | 2017-09-08 | 江苏中邦制药有限公司 | A kind of method for directly synthesizing nanometer small particle ZPT |
| CN107098824A (en) * | 2017-05-24 | 2017-08-29 | 河南心连心化肥有限公司 | The device and production method of a kind of utilization supergravity reactor production oxamides |
| CN107758672A (en) * | 2017-12-04 | 2018-03-06 | 中国恩菲工程技术有限公司 | The recovery method of silica flour in crystalline silicon cutting waste material |
| CN109053412A (en) * | 2018-08-13 | 2018-12-21 | 南京塔川化工设备有限公司 | Homogeneous premixing method before a kind of PTA energy saving device and CTA oxidation reaction |
| CN109053412B (en) * | 2018-08-13 | 2023-11-10 | 南京塔川化工设备有限公司 | PTA energy saving and consumption reducing device and homogeneous phase premixing method before CTA oxidation reaction |
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| CN110903179B (en) * | 2018-09-17 | 2022-05-24 | 中国石油化工股份有限公司 | Method for synthesizing acetone condensation compound by acetone and hydrogen |
| CN111082042A (en) * | 2018-10-21 | 2020-04-28 | 圣戈莱（北京）科技有限公司 | Ternary positive electrode material micron single crystal structure for lithium ion battery and preparation method thereof |
| CN109647315A (en) * | 2019-01-08 | 2019-04-19 | 北京化工大学 | Super-gravity device, method for oxidation and the system that energy makes full use of |
| CN111653796A (en) * | 2020-06-12 | 2020-09-11 | 清华大学 | Batch preparation method of uniform catalyst |
| CN114478614A (en) * | 2022-03-11 | 2022-05-13 | 新疆晶硕新材料有限公司 | Process and apparatus for the preparation of vinylchlorosilanes |
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