CN1243704C - Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization - Google Patents
Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization Download PDFInfo
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- CN1243704C CN1243704C CN 02136151 CN02136151A CN1243704C CN 1243704 C CN1243704 C CN 1243704C CN 02136151 CN02136151 CN 02136151 CN 02136151 A CN02136151 A CN 02136151A CN 1243704 C CN1243704 C CN 1243704C
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Abstract
The present invention relates to a method for preparing aromatic carboxylic acids by aralkyl oxidization and an oxidization reactor. The oxidization reactor comprises a combined stirring device, an oxidizing gas inlet device and a plurality of baffle plates, wherein the combined stirring device is axially arranged in a pressure container; the oxidizing gas inlet device is positioned between a middle stirring paddle and a lower stirring paddle, and adjacent to the lower stirring paddle; the baffle plates are vertically arranged on the inner wall of the reactor and provided with groove gaps, and gaps are reserved among the baffle plates and the inner wall of the reactor. The width of each baffle plate accounts for 0.06 to 0.1 of the inner diameter of the reactor. As the structure of the reactor is generally adjusted, including the stirring paddles, the baffle plates and the ventilation method, the mixing-dispersing performance of a three-phase system is obviously improved. The reaction material is rapidly and effectively dispersed, the particle size distribution is uniform, the gas processing capability is increased, and the gas containing rate is enhanced. As the partial non-uniform region disappears, the entire reaction space is effectively utilized, the production intensity of the reactor is enhanced, and the material consumption and the energy consumption are reduced.
Description
Technical field
The present invention relates to a kind of method of preparing arylcarboxylic acid by aralkyl oxidization, and the oxidation reactor that is adopted, specifically, relate to dimethylbenzene under cobalt, manganese, bromine catalyst effect, in acetate solvate, pass through the gas-liquid phase reaction with air or good fortune oxygen, p xylene oxidation is become method of terephthalic acid and the reactor that is adopted, particularly whipping appts in the reactor and the baffle plate that is arranged in the reactor.
Background technology
The oxidizing reaction of dimethylbenzene is a kind of complex reaction, removes the main reaction that generates terephthalic acid, and other has side reaction to generate multiple by product: as p-Hydroxybenzaldehyde, p-methylbenzoic acid and p-tolyl aldehyde etc.In addition, acetic acid can decompose, and dimethylbenzene and solvent acetic acid all can the generating unit divided combustions, generates CO, CO
2And water.Resultant of reaction is separated out with crystallization, is suspended in the system, Gu constitute gas-liquid-three-phase system.Reaction process will be emitted a large amount of heats.This reaction generally is being provided with venting port and is better carrying out in the blended stirred reactor.
Practice and theoretical investigation prove that all the admixture in the reactor will directly influence the efficient of oxidizing reaction and the quality of product, therefore, design and a kind ofly can carry out the target that well-mixed reactor has become numerous scientist and pursued to reaction mass.Chinese patent 89102155.8 has disclosed a kind of oxidation reactor that the aralkyl oxidation prepares aromatic carboxylic acid that is used for, the technology that this patent is reported is improved traditional technology, the oxidizing gas inlet is arranged on the bottom of whipping appts, width with baffle plate changes 0.02～0.04 of reactor inside diameter into by traditional 1/12 of reactor inside diameter that is about simultaneously, thereby increased the capacity of gas in the reactor and reduced energy consumption, this patent has adopted a kind of whipping appts that is provided with two-layer blade simultaneously.Because the baffle plate of this patent is too narrow, and general reactor aspect ratio is all bigger, even two layers of blade superpower also can not mix very.The bottom granule density is bigger, even assembles, deposits; Reactant can not effectively disperse rapidly, influences speed of reaction and products distribution, and by product is increased.The capacity of its gas can't satisfy the needs of reaction fully, and mixing of materials is even inadequately.As lower floor's blade is moved down, though can improve the mixing and the size distribution of bottom, enlarged the oar spacing, partial circulating between oar can appear; Move down as the upper strata blade, then the upper strata upper space particularly may cause more uneven distribution mutually near the free surface.Therefore a kind of new oxidation reactor for preparing aromatic carboxylic acid with energy-conservation aralkyl oxidation that mixes of development research is that institute of branch of industry is very expected.
Summary of the invention
One of technical issues that need to address of the present invention are the oxidation reactors that discloses a kind of preparing arylcarboxylic acid by aralkyl oxidization, can not satisfy the needs of reaction and mixing of materials defective uniformly inadequately fully with the capacity that overcomes the gas that prior art exists;
Two of the technical issues that need to address of the present invention provide a kind of method of preparing arylcarboxylic acid by aralkyl oxidization.
Technical scheme of the present invention:
The present invention is to the structure of traditional oxidation reactor, comprises that whipping appts, baffle plate and oxidizing gas entry position carried out comprehensively optimizing and revising, and this oxidation reactor comprises:
A round shape vertical pressure vessel that is provided with the material inlet device;
A combination whipping appts that axially is installed in the described pressurized vessel, the present invention selects three kinds of different oar types, constitute three layers of combination oar, described combination whipping appts comprises: near the wide leaf stirring rake of upper strata aerofoil profile axial flow that is positioned at the round shape vertical pressure vessel medium position, this oar power is lower and circulation ability is strong, has the better gas dispersive ability, to reach the purpose of homogeneous material; A near middle level remodeling turbine impeller that is positioned at the round shape vertical pressure vessel lower position, this stirring rake has stronger shearing force, ventilation back power does not descend substantially, to the processing power of gas be ordinary straight leaf turbine 2-4 doubly, gas dispersion when helping big air flow is so that gas effectively disperses; Near lower floor's stirring rake that is positioned at the round shape vertical pressure vessel bottom position, this lower floor's stirring rake employing good cycle, the aerofoil profile axial flow narrow leaf stirring rake that power is low are to guarantee that particle suspended the end of from.Special performance is separately given full play in the combination of three kinds of dissimilar blades, makes gas dispersion in the reactor, liquid mixing, and solid suspension, the mixing-dispersing property of three-phase system significantly improves.Reaction mass disperses quickly and effectively, even particle distribution, and gas processing capability increases, and gas holdup rises.Because local inhomogeneous district disappears, the entire reaction space is used more effectively, and improves the production intensity of reactor;
One for preventing to stop up, guarantee safety operation, the present invention takes the multitube sparger of annular distribution between middle level stirring rake and lower floor's stirring rake, near the oxidizing gas inlet device of lower floor's stirring rake, and air-flow is discharged downwards, and the pipe number is the 4-8 root;
A plurality ofly be vertically installed in reactor wall and leave the baffle plate gap, that be provided with the groove crack with reactor wall, the width of this baffle plate is 0.06～0.1 of a reactor inside diameter, the present invention reduces the width appropriateness of baffle plate, on baffle plate, slot simultaneously, make total width enough big, and span width is enough little, has both reduced systemic resistance, save energy consumption, avoid central whirlpool simultaneously.In two-phase and multiphase system, make the gas holdup increase reach 15-25%, over-all properties is better than stenotic baffle.
Since across-the-board regulation of the present invention the structure of reactor, comprise stirring rake, baffle plate and ventilating mode, the mixing-dispersing property of three-phase system significantly improves.Reaction mass disperses quickly and effectively, even particle distribution, and gas processing capability increases, and gas holdup rises.Because local inhomogeneous district disappears, the entire reaction space is used more effectively, and improves the production intensity of reactor, has reduced material consumption and energy consumption.
Description of drawings
Fig. 1 is the overall structure synoptic diagram of reactor of the present invention.
Fig. 2 is the stereographic map of upper strata stirring rake.
Fig. 3 is the top perspective view of middle level stirring rake.Fig. 4 is the front perspective view of middle level oar.
Fig. 5 is the top perspective view of lower floor's oar.
Fig. 6 is eight pipe ring formula gas distributor structural representations.
Fig. 7 is four pipe ring formula gas distributor structural representations.
Fig. 8 is single seam baffle plate synoptic diagram.
Fig. 9 double slit baffle plate synoptic diagram.
Figure 10 is the synoptic diagram of baffle plate end finger-type.
Figure 11 is the synoptic diagram of this production process.
Embodiment
See Fig. 1, oxidation reactor of the present invention comprises:
A round shape vertical pressure vessel 1 that is provided with material inlet device 2;
A whipping appts 3 that axially is installed in the described round shape vertical pressure vessel 1, described whipping appts 3 comprises: near 301, one of the wide leaf stirring rake of upper strata aerofoil profile axial flow that are positioned at round shape vertical pressure vessel 1 medium position is positioned near round shape vertical pressure vessel 1 lower position middle level remodeling turbine impeller 302 and one and is positioned near round shape vertical pressure vessel 1 bottom position lower floor's aerofoil profile axial flow narrow leaf stirring rake 303.
Aerofoil profile axial flow wide leaf stirring rake 301 in upper strata adopts the aerofoil profile axial flow square blade that is provided with 6 high expanded area ratio blades 311, central authorities are wheel hub, blade 311 is connected by floor with wheel hub, by wheel hub blade 311 is installed in the rotating shaft, described blade intersects formed section with cylindrical surface arbitrary and that its wheel hub is coaxial and is airfoil type in the width range of its radial direction, the expanded area ratio of axial flow oar is 0.15～1.2, expanded area ratio refer to blade with the vertical horizontal plane of rotating shaft on the ratio of shadow area sum inswept disk area when rotating with the aerofoil profile oar, as shown in Figure 2, concrete structure is disclosed by Chinese patent 92245125.7;
Middle level remodeling turbine impeller 302 adopts the remodeling turbine, comprise a disk 322 and 6 semicircles or the parabola shaped blade 323 that are arranged on these disk 322 outer rims, the width on blade 323 tops is than the width outstanding 15～50% of bottom, blade 323 evenly is installed on the centrifugal disc 322, and be connected with rotating shaft by disk 322, as shown in Figure 3 and Figure 4, concrete structure is disclosed by United States Patent (USP) 5791780;
Lower floor's aerofoil profile axial flow narrow leaf stirring rake 303 adopts the oblique oar of aerofoil profile axial flow narrow leaf, this stirring rake 303 has six low expanded area ratio blades 333, as shown in Figure 5, central authorities are wheel hub, blade 333 is connected by floor with wheel hub, by wheel hub blade 333 is installed in the rotating shaft, described blade intersects formed section with cylindrical surface arbitrary and that its wheel hub is coaxial and is airfoil type in the width range of its radial direction.Concrete structure is disclosed by Chinese patent 92245125.7.One of ordinary skill in the art can be made the whipping appts of being addressed easily according to the disclosed technology of above-mentioned patent;
Comparison diagram 2 and Fig. 5 as seen, the width of the blade 311 that the width of the blade 333 that lower floor's aerofoil profile axial flow narrow leaf stirring rake 303 adopts adopts less than the wide leaf stirring rake 301 of upper strata aerofoil profile axial flow.Therefore, aerofoil profile axial flow wide leaf stirring rake 301 in upper strata is also referred to as aerofoil profile axial flow square blade, and lower floor's aerofoil profile axial flow narrow leaf stirring rake 303 is also referred to as the oblique oar of aerofoil profile axial flow narrow leaf, that is the expanded area ratio of blade 311 is greater than the expanded area ratio of blade 333.
One between middle level stirring rake 302 and lower floor's stirring rake 303, near the oxidizing gas inlet device 4 of lower floor stirring rake 303, preferred inlet device 4 is a kind of pipe ring formula gas distributor, comprise annular distribution pipe 401 and coupled logical distribution arms 402, as Fig. 6 or shown in Figure 7, the mouth of pipe is downward, the arm number is the 4-8 root, evenly arrange along annular distribution pipe 401, the diameter of annular distribution pipe 401 is 0.8～1.5 times of diameter of lower floor's agitating vane 303, the width between centers of the arm mouth of pipe and impeller is 0.1～0.35T, and T is pressurized vessel 1 internal diameter;
A plurality of pressurized vessel 1 inwalls that are vertically installed in, vertical uniform distribution, and leave the gap with reactor wall, be provided with the baffle plate 5 in groove crack 501, from span from 0.008～0.012T, the width of this baffle plate 5 is 0.06～0.1 times of pressurized vessel 1 internal diameter, the quantity of baffle plate 5 is 4, groove crack 501 on the baffle plate 5 can be one, also can be many, the bottom of baffle plate is provided with finger-type 502, account for 10～25% of baffle plate total height, as Fig. 8, Fig. 9 and shown in Figure 10, the effect of finger-type 502 is that more effective elimination turns round and round, and the area in groove crack 501 is 10～35% times of baffle plate, and groove crack 501 can be arranged on the middle part of baffle plate 5, the inboard or the outside.
Preparing arylcarboxylic acid by aralkyl oxidization, producing terephthalic acid as p xylene oxidation can be 190-200 ℃ in temperature of reaction in above-mentioned oxidation reactor, reaction pressure is 13-15kg/cm
2Condition under, undertaken by the oxygen-containing gas liquid-phase oxidation p-Xylol in transpirable solvent medium.Figure 11 is the synoptic diagram of this production process.Pei Zhi reaction mass in advance, wherein contain the material inlet device 2 adding pressurized vessels 1 from pressurized vessel 1 middle part such as dimethylbenzene, acetic acid, water and catalyzer, oxygen-containing gas is introduced into the inside of pressurized vessel 1 by oxidizing gas inlet device 4, and liquid oxidation thing and solvent medium are drawn by material outlet device 6.This reaction is strong thermopositive reaction, relies on the evaporation of solvent acetic acid, removes heat.The acetic acid of a large amount of evaporations by condensation in the condenser 8 that is arranged on pressurized vessel 1 top after, returning pressure container 1, non-condensable gases and water are discharged from reactive system by pipeline 9.
Adopt above-mentioned method preparing arylcarboxylic acid by aralkyl oxidization, because the choose reasonable and the configuration of paddle wheel, coupling between impeller, baffle plate, the ventpipe, coordination, mixing time is shortened, gas holdup increases, particle suspension, and what is more important, component distributes in the reactor, distributing mutually more meets the needs of oxidizing reaction.In the simulation test of the different scales that is comparable to the industrial production condition, the good result that all shows the present invention and obtained.
Claims (6)
1. preparing arylcarboxylic acid by aralkyl oxidization reactor, comprise round shape vertical pressure vessel (1), be vertically installed in round shape vertical pressure vessel (1) inwall and leave the baffle plate (5) in gap, a whipping appts (3) and an oxidizing gas inlet device (4) that axially is installed in the round shape vertical pressure vessel (1), it is characterized in that with round shape vertical pressure vessel (1) inwall:
Said whipping appts (3) comprising:
Near the wide leaf stirring rake of upper strata aerofoil profile axial flow (301) that is positioned at round shape vertical pressure vessel (1) medium position, one is positioned near round shape vertical pressure vessel (1) lower position middle level remodeling turbine impeller (302) and one and is positioned near the lower floor's aerofoil profile axial flow narrow leaf stirring rake (303) of round shape vertical pressure vessel (1) bottom position;
Said oxidizing gas inlet device (4) is positioned between middle level stirring rake (302) and the lower floor's stirring rake (303), close lower floor stirring rake place; Oxidizing gas inlet device (4) is taked the multitube sparger of annular distribution, and air-flow is discharged downwards, and the pipe number is the 4-8 root;
Said baffle plate (5) is provided with groove crack (501), and the width of baffle plate (5) is 0.06～0.1 times of pressurized vessel (1) internal diameter, and the bottom of baffle plate is provided with finger-type (502).
2. reactor as claimed in claim 1, it is characterized in that: the wide leaf stirring rake of upper strata aerofoil profile axial flow (301) adopts the aerofoil profile axial flow square blade that is provided with 6 blades (311), central authorities are wheel hub, blade (311) is connected by floor with wheel hub, by wheel hub blade (311) is installed in the rotating shaft, described blade intersects formed section with cylindrical surface arbitrary and that its wheel hub is coaxial and is airfoil type in the width range of its radial direction, the expanded area ratio of axial flow oar is 0.15～1.2, expanded area ratio refer to blade with the vertical horizontal plane of rotating shaft on the ratio of shadow area sum inswept disk area when rotating with the aerofoil profile oar;
Middle level remodeling turbine impeller (302) adopts the remodeling turbine, comprise a disk (322) and be arranged on 6 semicircles or the parabola shaped blade (323) of this disk (322) outer rim, the width on blade (323) top is than the width outstanding 15～50% of bottom, blade (323) evenly is installed on the centrifugal disc (322), and is connected with rotating shaft by disk (322);
Lower floor's aerofoil profile axial flow narrow leaf stirring rake (303) adopts the oblique oar of aerofoil profile axial flow narrow leaf, this stirring rake (303) has six blades (333), central authorities are wheel hub, blade (333) is connected by floor with wheel hub, by wheel hub blade (333) is installed in the rotating shaft, described blade intersects formed section with cylindrical surface arbitrary and that its wheel hub is coaxial and is airfoil type in the width range of its radial direction;
The expanded area ratio of blade (311) is greater than the expanded area ratio of blade (333).
3. reactor as claimed in claim 1, it is characterized in that: said inlet device (4) comprises annular distribution pipe (401) and coupled logical distribution arms (402), the mouth of pipe is downward, the arm number is the 4-8 root, evenly arrange along annular distribution pipe (401), the diameter of annular distribution pipe (401) is 0.8～1.5 times of diameter of lower floor's agitating vane (303), and the width between centers of the arm mouth of pipe and impeller is 0.1～0.35T, and T is pressurized vessel (a 1) internal diameter.
4. reactor as claimed in claim 1 or 2, it is characterized in that: the groove crack (501) on the baffle plate (5) can be one or more, the area in groove crack (501) is 10～35% of a baffle plate, groove crack (501) is arranged on middle part, inboard or the outside of baffle plate (5), gap between baffle plate (5) and the reactor wall is 0.008～0.012T, and T is pressurized vessel (a 1) internal diameter.
5. reactor as claimed in claim 4 is characterized in that: the finger-type (502) of baffle plate (5) bottom accounts for 10～25% of baffle plate total height.
6. the method for a preparing arylcarboxylic acid by aralkyl oxidization, it is characterized in that: this method is included in the arbitrary described oxidation reactor of claim 1～5, by the reactions steps of the oxygen-containing gas liquid-phase oxidation p-Xylol in transpirable solvent medium.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136151 CN1243704C (en) | 2002-07-22 | 2002-07-22 | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization |
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|---|---|---|---|
| CN 02136151 CN1243704C (en) | 2002-07-22 | 2002-07-22 | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization |
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| CN1390823A CN1390823A (en) | 2003-01-15 |
| CN1243704C true CN1243704C (en) | 2006-03-01 |
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| CN103146564A (en) * | 2012-12-03 | 2013-06-12 | 华东理工大学 | Coaxial different-speed combined oar reactor and industrial application thereof |
| CN103223325A (en) * | 2013-05-07 | 2013-07-31 | 南通大力化工设备有限公司 | Mechanical agitator of reaction vessel |
| CN104707510B (en) * | 2013-12-13 | 2017-01-18 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and polymer solution processing method |
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| KR102256402B1 (en) * | 2018-10-15 | 2021-05-25 | 한화솔루션 주식회사 | Batch reactor |
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| CN109806835B (en) * | 2019-01-31 | 2024-01-05 | 森松（江苏）重工有限公司 | Novel PTA oxidation reactor |
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