CN101092350B - Oxidizing reactor in bubbling tower of internal circulation for producing aromatic acid - Google Patents
Oxidizing reactor in bubbling tower of internal circulation for producing aromatic acid Download PDFInfo
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- CN101092350B CN101092350B CN2007100246355A CN200710024635A CN101092350B CN 101092350 B CN101092350 B CN 101092350B CN 2007100246355 A CN2007100246355 A CN 2007100246355A CN 200710024635 A CN200710024635 A CN 200710024635A CN 101092350 B CN101092350 B CN 101092350B
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Abstract
This invention relates to an inner circulating bubbling column oxidation reactor for producing aromatic acids. The column is composed of three sections, i.e., a gas-liquid separation section at the upper part, a multi-stage bubbling section at the middle part and a solid-liquid suspension section at the lower part. The multi-stage bubbling section is equipped with 1-5 stage gas distributor and 1-5 stage inner circulating draft-tube. The reactor is free of any moving part inside, and can promote raw material circulation in a certain region in the column, effectively eliminate inadequate mixing zone, and obviously decrease raw material concentration and temperature gradient by synergistic effect of inner circulating draft-tube and gas distributor.
Description
Technical field
The present invention relates to technological method and reaction unit that the aromatic hydrocarbon liquid-phase oxidation prepares aromatic acid, relate in particular to a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, belong to technical field of chemical.
Background technology
Bubbling column reactor is the important device that gas-liquid two-phase or gas-liquid-solid three-phase are carried out quality, energy and chemical reaction, has characteristics simple in structure, stable operation.The aromatic hydrocarbon liquid-phase oxidation prepares the technological method of aromatic acid, the industrial bubbling column reactor that adopts, and particularly the p-Xylol liquid phase catalytic oxidation prepares terephthalic acid, and the trend of more and more large-scale change is arranged in recent years.
The most employing of commercial-scale terephthalic acid preparation technology acetic acid is solvent, cobalt, manganese, bromine compounds are composite catalyst, air or oxygen rich air are oxygenant, entering oxidation reactor continuously with the raw material p-Xylol reacts, in typical case, 155～225 ℃ of temperature of reaction, reaction pressure 0.5～3.0MPa, the residence time 30～120min.Reaction heat is withdrawn from condensate return reactor by evaporation, the condensation of solvent acetic acid; Thick product terephthalic acid is separated out at the reactor intercrystalline, is continuously removed reactor in the mode of slurry.
According to this technology, the material system of p-Xylol liquid-phase catalytic oxidation device of preparation terephthalic acid is " gas (air, acetic acid steam)-liquid (acetic acid, p-Xylol) solid-(terephthalic acid) " three-phase state, and the design of oxidation reactor must satisfy simultaneously that air dispersion, liquid phase material are mixed, the requirement of solid particulate suspension.In the prior art, commercial-scale p-Xylol liquid-phase oxidation reactor comprises stirring reactor and bubbling column reactor two classes.
The synergy of the oblique leaf oar combination of leaf stirring rake and lower floor's upper-turn-type that U.S. Pat P5211924, USP5102630 and Chinese patent ZL89102155 adopt the air distributing nozzle, the upper strata is straight, narrow baffle plate realizes mixing of materials in Gas-Liquid Dispersion and the still.Japanese Patent Publication 61-21217 utilizes special broach shape paddle wheel to improve Gas-Liquid Dispersion; Japanese Patent Publication 47-14092 imports the agitating vane of raw material p-Xylol from hollow, has promoted the raw material mixing.All in all, stirring reactor mechanism complexity is safeguarded inconvenient.
Patent CN1228302C and patent CN1680250A disclose the uniform up and down straight barrel type bubble tower reaction unit of producing aromatic carboxylic acid, patent CN1785495A is provided with damping internal construction member in bubbling column reactor, to suppress the too fast flow velocity in central zone in the tower, interference flowing field improves gas-liquid mass transfer speed simultaneously.Patent CN1208301C discloses a kind of air lift type outer circulation bubble tower oxidation unit that terephthalic acid is used of producing, utilize urceolus that tower top slurry is introduced lower region by the gas lift effect, form the circulation of fluid at full tower, improve temperature and concentration distribution in the tower, and adopt bigger aspect ratio to strengthen gas-liquid mass transfer.But the top oxygen concentration of larger ratio of height to diameter bubble tower is lower, influences reaction efficiency.
Patent CN1293184 is from changing the angle of the flow-pattern of material reactor, make to be reflected in the tower reactor and carry out with flow-pattern near piston flow, improving p xylene oxidation is the speed and the transformation efficiency of terephthalic acid, the internal structure more complicated of its reactor.
Patent disclosure CN1807392A has proposed a kind of tower oxidation reaction apparatus of bubbling that p xylene oxidation prepares terephthalic acid that is used for, at the sidewall of lower reaction section equally distributed 2～8 phase feed are set circumferentially and divide import, attempt to strengthen Gas-Liquid Dispersion by the multiple spot air inlet.
Summary of the invention
The oxidizing reactor in bubbling tower of internal circulation that the purpose of this invention is to provide a kind of production aromatic acid simple in structure is to overcome the defective of above-mentioned many pre-existing reactors of enumerating.
For realizing purpose of the present invention, a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, its tower body is made up of the gas-liquid separation section on top, the multistage bubbling segment at middle part, solid-liquid suspension section three parts of bottom, it is characterized in that: the multistage bubbling segment inside at this reactor middle part is equipped with 1～5 grade of gas distributor and 1～5 grade of internal recycle guide shell.
Further, above-mentioned a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, wherein, described gas distributor becomes configuration set with the internal recycle guide shell, preferred 2～4 groups.
Further, above-mentioned a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, wherein, the sectional area of described internal recycle guide shell is 1/2～1/12 with the ratio of the sectional area of bubble tower, and the height of internal recycle guide shell is 1～3 with the ratio of the diameter D of bubble tower.
Further, above-mentioned a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, wherein, the cross-sectional shape of described internal recycle guide shell is circle or Polygons.
Again further, above-mentioned a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, wherein, the lower curtate of this bubbling column reactor is provided with bottom entering type agitator, and the top is provided with gas-liquid separator.
Like this, the present invention just proposes a kind of bubbling tower of internal circulation formula oxidation reactor simple in structure, its inside is without any moving parts, synergy by internal recycle guide shell and gas distributor, promote the material circulation of regional area in the tower, multistage air intake structure has obviously improved the axial oxygen concentration gradient of larger ratio of height to diameter bubble tower in the prior art, simple upright guide shell structure also can not cause the deposition of solid particulate, Flow of Goods and Materials in the guide shell is for falling the design of liquid stream, make the diameter of guide shell significantly reduce, effectively saved precious metal material, These characteristics makes this oxidation reactor have good application prospects at the aromatic acid production field.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 a/2b is the comparative analysis that the Fluid Mechanics Computation (CFD) of liquid phase flow in the bubbling column reactor is calculated, Fig. 2 a is the interior liquid speed distribution plan of the bubble tower of twin-stage internal recycle guide shell and gas distributor combination, and Fig. 2 b is the interior liquid speed distribution plan of the conventional bubble tower of no internal recycle guide shell.
Among the figure: 1-liquid phase feeding mouth, 2-slurry outlet, 3-gas inlet, 4-gas-liquid separation section, 5-internal recycle guide shell, 6-tower body, 7-gas distributor.
Embodiment
In the bubble column oxidation reactor of routine, after the gas distributor of gas by reactor bottom enters reactor, bubble constantly rising, coalescence, grow up, form large diameter bubble in the middle and upper part of reactor, though this has the higher apparent gas holdup, liquid-gas interface amasss and the middle and lower part of gas-liquid mass transfer ability not as bubbling column reactor.On the other hand, the inside of no inner member bubble tower, there is concentration difference in the liquid phase flow confusion in tower height degree direction, and the import and export operated by rotary motion of liquid-solid phase material causes bubble tower top reaction efficiency to reduce at the hypomere of tower.For the bubble tower of larger ratio of height to diameter, the problems referred to above are more outstanding.
The present invention adopts and the method for internal recycle guide shell rationally is set to solve the problems of the technologies described above in bubble tower.This bubble column oxidation reactor is made up of the gas-liquid separation section on top, the multistage bubbling segment at middle part, solid-liquid suspension section three parts of bottom, and the different heights in bubbling segment is equipped with the internal recycle guide shell of 1～5 grade of gas distributor and 1～5 grade.
Reasonable disposition internal recycle thrust-augmenting nozzle in the bubble tower, under the synergy of gas distributor, the flow principles of inducing based on outside difference of gas holdup and gas distributor exit gas in the thrust-augmenting nozzle, the inside and outside gas-liquid that formed of guide shell circulates, and has effectively promoted the back-mixing of regional area in the bubble tower.During work, the feed-pipe from reactor lower part after the aromatic hydrocarbon raw material of liquid phase, solvent, the catalyst mix adds; Air or oxygen rich air enter from the gas distributor of reactor lower part, and gas disperses the back bubbling to enter the liquid phase reaction district through sparger.The work off one's feeling vent one's spleen guiding of burble of control sparger, make the outside of the guide shell that places the bubbling reactor center have higher gas holdup, because the apparent density difference that guide shell is inside and outside, liquid-solid slurry in the guide shell just flows under action of gravity from top to bottom, the material on guide shell top is constantly turned back to the bottom of guide shell, form circulation and effectively eliminate bad mixing zone, material concentration and thermograde are reduced.The cycling stream that guide shell forms also helps to suppress the generation of air pocket.
For the bubble column oxidation reactor of larger ratio of height to diameter, multistage internal recycle guide shell and multistage gas distributor can be set, with each regional liquid phase circulatory problems in the collaborative solution tower.The multistage of air or oxygen rich gas enters, and also helps larger ratio of height to diameter bubble column oxidation reactor top oxygen replenishment, impels the full tower homogenizing of oxidizing reaction, improves the space time yield of reactor.
As shown in Figure 1, the main body of oxidizing reactor in bubbling tower of internal circulation of the present invention is a tower body 6, its inside can be divided into: solid-liquid suspension section three parts of the gas-liquid separation section 4 on top, the multistage bubbling segment at middle part, bottom, the multistage bubbling segment at middle part is provided with internal recycle guide shell 5 and gas distributor 7.During work, liquid aromatic hydrocarbons, solvent, catalyzer enter reactor from the opening for feed 1 of bubble tower bottom, air or oxygen rich gas 3 enter from entering the mouth, and entering reaction zone after disperseing through gas distributor 7, and the product slurry leaves reactor from the slurry outlet 2 of reactor bottom.
Lower curtate at this reactor can be provided with bottom entering type agitator, to prevent the deposition of slurry; Oxidation reaction heat is removed by the mode of solvent evaporation, and the top of reactor is provided with gas-liquid separator 4 to suppress liquid foam entrainment.For the bubble column oxidation reactor of larger ratio of height to diameter, the different heights in bubbling segment is installed multistage gas distributor 7 and multistage internal recycle guide shell 5, and gas distributor 7 can become configuration set with internal recycle guide shell 5, preferential 2～4 groups.
Below main points of the present invention are described in further detail.
1, gas distributor
Gas distributor among the present invention can be ring-type porous sparger or multitube mouth sparger, also can be the sparger of other industrial common type.Gas distributor is installed in the below of internal recycle guide shell, and pneumatic outlet places between circulation guide shell and the tower wall.Like this, bubble flow enters the ring-like passage between the guide shell outside and the bubble tower wall, and the downward liquid flowing rate in the guide shell is strengthened in the action of gravity of collaborative liquid.
2, the aspect ratio of bubble tower
The aspect ratio of bubble tower is little to make easily that gas short circuit, aspect ratio cause easily greatly again in the tower that axial mixing of materials is bad, concentration distribution and temperature distribution inhomogeneous.Generally in 5, the aspect ratio of the bubble tower of band outer circulating tube is generally 7～10 for the aspect ratio of common bubble tower.The combination of multistage internal recycle guide shell and gas distributor can improve gas short circuit and axial mixed problem, thereby the bubble tower of suitable relative broad range aspect ratio, the aspect ratio that the present invention is suitable for is 5～12,1～5 grade of gas distributor of different heights installation in bubbling segment and 1～5 grade internal recycle guide shell.The air flow of gas distributors at different levels can be controlled respectively, the preferential principle that progressively reduces from bottom to top that adopts.
3, internal recycle guide shell
The function of the internal recycle guide shell among the present invention is to utilize the gas holdup difference in the outside in the guide shell, causing circulating of liquid phase inside and outside the guide shell under the effect of gravity.Especially, the work off one's feeling vent one's spleen guiding of burble of control sparger makes the outside of the guide shell that places the bubbling reactor center have higher gas holdup, liquid-solid slurry in the guide shell just flows under action of gravity from top to bottom, the material on guide shell top is constantly turned back to the bottom of guide shell, form circulation and effectively eliminate bad mixing zone, material concentration and thermograde are reduced.
The sectional area of internal recycle guide shell has determined the flow of liquid phase cycling stream.The superiority that the interior liquid of guide shell flows to the design of current downflow is: obtain under the identical liquid phase cycling stream prerequisite, its sectional area gas-liquid flow in the guide shell upwards flows, the design of guide shell outside liquid under flowing to, significantly save the material cost and convenient installation of guide shell, outstanding especially for large-scale bubbling column reactor; On the other hand, the existence of internal recycle guide shell has changed flowing of bubble tower central zone, avoided conventional bubble tower center gas excessive, the problems such as the residence time is too short, bubble coalescence of speed that flow, the flow rate of the gas-liquid flow between the guide shell outside and the bubble tower wall is even.The ratio that the present invention proposes internal recycle guide shell sectional area and bubble tower sectional area is 1/2～1/12; Internal recycle guide shell cross-sectional shape can be circle or Polygons, and is preferably circular; The height of internal recycle guide shell is 1～3 with the ratio of the diameter D of bubble tower.
Below in conjunction with specific examples technical solution of the present invention is described further.These examples only are some exemplary applications, can not be interpreted as a kind of restriction to claim protection domain of the present invention.
A kind of representative instance of the present invention is the bubbling column reactor of twin-stage inner draft tube and gas distributor combination: reactor inside diameter 380mm, the straight tube height of reactor 2000mm; Inner draft tube internal diameter 100mm, inner draft tube height 500mm; The gas distributor that twin-stage 4 straight tubes symmetry is uniform, straight tube internal diameter 25mm, depth of penetration 25mm; The interlamellar spacing 1400mm of twin-stage gas distributor, the inner draft tube lower edge be higher than with respect to gas distributor 200mm; Levels sparger air input is respectively 10m
3/ h and 30m
3/ h.
As a comparison, the bubbling column reactor of no inner draft tube: reactor inside diameter 380mm, the straight tube height of reactor 2000mm; The gas distributor that individual layer 4 straight tubes symmetries is uniform, straight tube internal diameter 25mm, depth of penetration 25mm, the mouth of pipe apart from the limit wall apart from 25mm; Air flow 40m
3/ h.
The Fluid Mechanics Computation (CFD) in the interior liquid phase flow field of bubble tower was simulated comparative analysis shown in Fig. 2 a and Fig. 2 b when whether the internal recycle guide shell of above-mentioned specific examples existed: Fig. 2 a is the interior liquid speed distribution of the bubble tower of twin-stage internal recycle guide shell and gas distributor combination, and Fig. 2 b is the interior liquid speed distribution of the conventional bubble tower of no internal recycle guide shell.
Fig. 2 a and Fig. 2 b comparing result show: rationally be provided with in the bubble tower after the internal recycle guide shell, liquid phase flow has obtained obvious improvement, and the liquid phase flow in the full tower is even, flow velocity strengthens, the flow field is regular; The liquid rule flows downward in the guide shell, has strengthened the mixing of bubble tower axial flow of fluid, promotes the homogenizing of concentration gradient and thermograde; Because the downward liquid stream in the guide shell has been induced flowing of tower lower flow; Guide shell has suppressed the gas-liquid upper reaches of tower central section, thereby has also improved guide shell top liquid phase flow.
In a word, the present invention proposes a kind of bubbling tower of internal circulation formula oxidation reactor simple in structure, easy to implement, its inside is without any moving component, synergy by interior circulation guide shell and gas distributor, promote the Matter Transfer of regional area in the tower, the Multi-stage inlet structure has obviously been improved the axial oxygen concentration gradient of larger ratio of height to diameter bubble tower in the prior art, simple upright guide shell structure also can not cause the deposition of solid particle, Flow of Goods and Materials in the guide shell is for falling the design of liquid stream, so that the diameter of guide shell significantly reduces, effectively saved precious metal material. These characteristics make the present invention at the aromatic acid production field good application prospect be arranged.
Claims (6)
1. oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid, its tower body is made up of the gas-liquid separation section on top, the multistage bubbling segment at middle part, solid-liquid suspension section three parts of bottom, it is characterized in that: the multistage bubbling segment inside at this reactor middle part is equipped with 1～5 grade of gas distributor and 1～5 grade of internal recycle guide shell.
2. a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid according to claim 1 is characterized in that: described gas distributor becomes configuration set with the internal recycle guide shell, and quantity in groups is 2～4 groups.
3. a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid according to claim 1 and 2, it is characterized in that: the sectional area of described internal recycle guide shell is 1/2～1/12 with the ratio of the sectional area of bubble tower, and the height of internal recycle guide shell is 1～3 with the ratio of the diameter D of bubble tower.
4. a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid according to claim 1 and 2 is characterized in that: the cross-sectional shape of described internal recycle guide shell is circle or Polygons.
5. a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid according to claim 1 and 2, it is characterized in that: the bottom of this bubbling column reactor is provided with bottom entering type agitator.
6. a kind of oxidizing reactor in bubbling tower of internal circulation of producing aromatic acid according to claim 1 and 2, it is characterized in that: the top of this bubbling column reactor is provided with gas-liquid separator.
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| CN2007100246355A CN101092350B (en) | 2007-06-26 | 2007-06-26 | Oxidizing reactor in bubbling tower of internal circulation for producing aromatic acid |
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|---|---|---|---|
| CN2007100246355A CN101092350B (en) | 2007-06-26 | 2007-06-26 | Oxidizing reactor in bubbling tower of internal circulation for producing aromatic acid |
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| CN101092350A CN101092350A (en) | 2007-12-26 |
| CN101092350B true CN101092350B (en) | 2010-07-14 |
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| EP2336270A4 (en) | 2008-09-30 | 2012-03-07 | Japan Oil Gas & Metals Jogmec | METHOD FOR SYNTHESIZING LIQUID FUEL AND APPARATUS FOR SYNTHESIZING IT |
| CN106323706B (en) * | 2015-07-03 | 2019-05-07 | 中国石油化工股份有限公司 | The device and extraction equipment of oil content are collected from the liquid carbon dioxide dissolved with oil content |
| CN108675433A (en) * | 2018-06-22 | 2018-10-19 | 杭州深瑞水务有限公司 | A kind of multistage air inlet wet oxidation system |
| CN114307935B (en) * | 2022-01-06 | 2023-03-28 | 南京工业大学 | Air-lift reactor with self-suction aeration structure |
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Effective date of registration: 20160223 Address after: 211900 Yizheng Changjiang Road, Jiangsu, China, No. 1, No. Patentee after: CHINA SINOPEC YIZHENG CHEMICAL FIBER CO., LTD. Address before: 211900 No. 1 Changjiang West Road, Xu Town, Jiangsu City, Yizheng Province Patentee before: Yizheng Chemical Fiber Co., Ltd., China Petrochemical Group Corp. |