CN115007099B - Oxo reactor and working method thereof - Google Patents
Oxo reactor and working method thereof Download PDFInfo
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- CN115007099B CN115007099B CN202210586906.0A CN202210586906A CN115007099B CN 115007099 B CN115007099 B CN 115007099B CN 202210586906 A CN202210586906 A CN 202210586906A CN 115007099 B CN115007099 B CN 115007099B
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/10—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide
- C07C51/12—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide on an oxygen-containing group in organic compounds, e.g. alcohols
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses an oxo reactor and a working method thereof, wherein the oxo reactor comprises a reactor shell, at least one liquid inlet tangential to the shell, a top liquid inlet, a gas outlet, a CO inlet, a circulating liquid outlet and a reaction liquid outlet; a nozzle is arranged at the end part of the top liquid inlet; the end of the CO inlet is provided with a nozzle. The invention realizes the uniform distribution of CO gas and raw material liquid in the reaction kettle by the matching of CO gas pulse opposite spraying and mixed liquid vortex motion, avoids the problem of mechanical seal leakage caused by mechanical stirring, reduces the equipment maintenance cost, enhances the gas-liquid mixed mass transfer effect in the reactor, improves the reaction rate and the raw material utilization rate, and ensures the long-term stable operation of the device.
Description
Technical Field
The invention relates to the technical fields of petrochemical industry and coal chemical industry, in particular to a oxo synthesis reactor and a working method thereof.
Background
Acetic acid is an important chemical intermediate and chemical product, and is mainly used for producing vinyl acetate monomer, terephthalic acid, acetate esters, acetic anhydride, halogenated acetic acid, cellulose acetate and other acetic acid derivatives. In addition, the acetic acid can be further processed into various products such as pesticides, medicines, dyes, synthetic fibers, adhesives and the like. The methanol oxo synthesis method is a main method for industrially producing acetic acid, wherein acetic acid is synthesized by liquid-phase methanol feed and gas-phase CO feed in a catalyst system, and the acetic acid produced by the method accounts for more than 80% of the total global acetic acid yield and becomes a main process for producing acetic acid. The traditional reactor for synthesizing acetic acid by carbonyl adopts mechanical stirring, because the methanol carbonyl reaction is a strong corrosion environment, equipment is easy to corrode and imported zirconium materials are needed, the manufacturing and maintenance cost of the stirring kettle is higher, meanwhile, the mechanical stirring has the problems of large vibration and easy leakage in sealing, the long-term stable and safe operation is difficult, and a gas-liquid mixing means for replacing the stirring kettle needs to be found.
In response to this problem, in recent years, the use of fluid agitation instead of mechanical agitation has been an important improvement. It is known from the patents CN202020145192.6 and CN202110014036.5 that the reaction raw material and the circulating mother liquid can be mixed by combining the reaction circulating liquid sprayed from a plurality of reducing nozzles near the wall with a gas distributor instead of mechanical stirring. In the patent CN201320103329.1 and CN201310072175.9, the central nozzle at the bottom of the reaction kettle can mix the gas phase and the liquid phase under the action of the annular gas distributor, so as to promote mass transfer of the gas phase and the liquid phase, but the vertical upward jet flow has limited dispersion of bubbles in the radial direction, and the effect is not ideal. CN201811224192.9, at least two nozzles close to the inner wall are disposed at the top of the reaction kettle, and a gas distributor is disposed at the bottom of the reaction kettle to achieve the purpose of fluid stirring. Eccentric setting of the spray head produces bias flow phenomenon, and gas-liquid dispersion in the reactor is uneven, and stirring effect is poor than that of a traditional stirring kettle.
In summary, the currently used fluid stirring technology has a poor stirring effect compared with the traditional mechanical stirring technology, low gas-liquid mixing degree and low device production efficiency.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide the oxo-synthesis reactor and the working method thereof, and by adopting the reactor provided by the invention, the leakage problem of mechanical seal existing in mechanical stirring can be avoided, the equipment maintenance cost is reduced, the gas-liquid mixed mass transfer effect in the reactor can be enhanced, the reaction rate and the raw material utilization rate are improved, and the aim of long-term safe and stable operation of the device is realized.
The invention can be realized by the following technical scheme:
the invention provides a oxo synthesis reactor, which comprises a reactor shell, at least one liquid inlet tangential to the shell, a top liquid inlet, a circulating liquid outlet, a reaction liquid outlet, a gas outlet and two CO inlets; the end parts of the two CO inlets, which are positioned in the reactor shell, are respectively provided with a first nozzle and a second nozzle; the outlets of the first nozzle and the second nozzle are arranged in opposite directions and are positioned on the same vertical line.
As a preferable scheme of the invention, the CO flow rates at the outlets of the first nozzle and the second nozzle are periodically changed at a certain pulse frequency, and a phase difference pi exists between the two.
As a preferred embodiment of the invention, the end of the liquid inlet in the reactor shell is provided with a third nozzle; the outlets of the first nozzle and the third nozzle are vertically downward, and the outlet of the second nozzle is vertically upward.
As a preferable scheme of the invention, the outlet of the third nozzle is positioned at a height which is 0.1-0.5 times the liquid level below the liquid level.
As a preferred embodiment of the present invention, the liquid inlet is disposed at a height between the first nozzle and the second nozzle.
As a preferred embodiment of the present invention, the number of the liquid inlets is 3, and the liquid inlets are located at the same height of the reactor shell, and the number of the liquid inlets is 120 ° from each other in the circumferential direction.
As a preferable scheme of the invention, the 3 liquid inlets are respectively a methanol liquid inlet, a catalyst mother liquor liquid inlet and a dilute acid mixed liquid inlet.
As a preferable scheme of the invention, the reactor shell consists of a reaction kettle cylinder body and upper and lower hemispherical/ellipsoidal heads.
As a preferable scheme of the invention, the distance between the first nozzle and the second nozzle is 0.01-0.2 times of the diameter of the reaction kettle.
In a preferred embodiment of the invention: the circulating liquid outlet and the reaction liquid outlet are positioned below the liquid inlet tangential to the shell.
Preferably, the recycle outlet is located at the bottom of the reactor.
The technical scheme of the invention is as follows: the liquid inlet tangential to the shell is positioned at 1/2-1/3 of the barrel from the bottom.
The technical scheme of the invention is as follows: and a spinning device is arranged on the liquid inlet tangential to the shell.
Preferably, the radial thickness of the spinning jack is 0.03-0.2 times of the diameter of the reaction kettle.
Preferably, the diameter of the nozzle at the end part of the CO inlet is 0.01-0.1 times of the diameter of the reaction kettle.
Preferably, the nozzle spacing of the end nozzle of the CO inlet is 0.01-0.2 times of the diameter of the reaction kettle.
In the technical scheme of the invention, the CO flow at the outlet of the nozzle at the end part of the CO inlet changes at a certain pulse frequency, and the CO flow have a phase difference pi.
Preferably, the CO flow rate variation frequency is 2-20 Hz.
In the technical scheme of the invention, the port nozzle of the top liquid inlet is positioned below the liquid level.
Preferably, the port nozzle of the top liquid inlet is located at a liquid level height of 0.1 to 0.5 times below the liquid level.
Preferably, the nozzle flow rate at the end of the CO inlet is 8-25 m/s.
Preferably, the nozzle flow rate at the top liquid inlet end is 8-25 m/s.
Preferably, the flow rate of the liquid in the cyclone is 5-15 m/s.
The invention also provides a oxo synthesis method based on the reactor, which comprises the following steps:
CO gas enters the reactor from two CO inlets and is sprayed at a first nozzle and a second nozzle; the CO flow at the outlets of the first nozzle and the second nozzle is periodically changed at a certain pulse frequency, and the two have a phase difference pi, so that the sputtered CO gas swings up and down due to the change of the flow of the first nozzle and the second nozzle, a large number of CO small bubbles are generated, and the CO gas is promoted to be uniformly distributed in the whole reaction kettle;
the methanol, the catalyst mother liquor and the dilute acid mixed liquor enter the reactor from three liquid inlets along the tangential direction of the shell; the gas flows in a vortex manner under the action of the cyclone, moves tangentially with CO small bubbles, and the bubbles are sheared to form smaller bubbles, so that the gas-liquid mass transfer process is facilitated;
the mixed liquid is stirred by the top methanol liquid jet flow, so that CO gas is uniformly distributed, and simultaneously, the sinking methanol liquid and the ascending CO gas move up and down mutually and are uniformly mixed, and the improvement of the reaction rate is facilitated.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, CO gas pulse counter-spraying is adopted, the mixed liquid flows in a vortex manner, and the methanol feed liquid is stirred in a jet manner and is matched with the cyclone, so that the distribution of CO gas and raw material liquid in the reaction kettle is improved. The whole reaction kettle is not provided with the traditional stirring component, so that the problem of leakage of a mechanical seal caused by mechanical stirring is solved, the safe operation of the device is ensured, the maintenance and replacement of the stirring kettle are avoided, the maintenance cost is reduced, and the power consumption of the device is reduced. And the micro bubbles are formed by opposite spraying of high-speed gas, and under the shearing action of vortex liquid, the bubbles in the reaction kettle are further reduced, so that the gas-liquid mass transfer efficiency and rate are improved, and the productivity is improved.
Drawings
FIG. 1 is a schematic diagram of a oxo reactor according to the present invention.
Fig. 2 is a schematic structural view of a spinning machine according to the present invention.
Fig. 3 is a schematic view of a nozzle structure according to the present invention.
Wherein: 1-a reactor shell; 2-a spinning device; 3-a liquid inlet tangential to the housing; 4-a reaction liquid outlet; 5-a circulating liquid outlet; 6-upper CO inlet; 7-a lower CO inlet; 8-third nozzle (top liquid inlet end nozzle); 9-gas outlet; 10-top liquid inlet; 11-first nozzle (upper CO inlet end nozzle); 12-second nozzle (lower CO inlet end nozzle).
Detailed Description
The oxo reactor provided by the present invention is further described below with reference to examples, but the scope of the present invention is not limited thereto:
FIG. 1 shows a oxo reactor according to the invention, comprising a reactor shell 1, a rotor 2, at least one liquid inlet 3 tangential to the shell, a reaction liquid outlet 4, a recycle liquid outlet 5, an upper CO inlet 6, a lower CO inlet 7, a gas outlet 9, a top liquid inlet 10; the reactor main body consists of a reaction kettle cylinder body and an upper hemispherical/ellipsoidal seal head and a lower hemispherical/ellipsoidal seal head; the number of the liquid inlets 3 is 3, namely a methanol liquid inlet, a catalyst mother liquor liquid inlet and a dilute acid mixed liquor liquid inlet, which are positioned at the same height of the reactor shell and form 120 degrees with each other, wherein the liquid inlets are tangential to the shell; a third nozzle 8 is arranged at the port of the top liquid inlet in the reaction kettle; the port of the upper CO inlet in the reaction kettle is provided with a first nozzle 11; the port of the lower CO inlet in the reaction kettle is provided with a second nozzle 12; the outlets of the third nozzle 8 and the first nozzle 11 are vertically downward, the outlet of the second nozzle 12 is vertically upward, and the first nozzle 11 and the second nozzle 12 are arranged in opposite directions and are positioned on the same vertical line; the liquid inlet 3 is axially positioned between the first nozzle 11 and the second nozzle 12; the CO flow rates at the outlets of the first nozzle 11 and the second nozzle 12 are periodically changed at a certain frequency, and a phase difference pi exists between the two, and the change periods of the two are the same. The circulating liquid flows out from the circulating liquid outlet 5, is cooled by an external circulating heat exchanger and then returns to the reaction kettle through the top liquid inlet 10 or the liquid inlet 3; the methanol raw material liquid, the catalyst mother liquid and the dilute acid mixed liquid respectively enter the reactor from three liquid inlets 3 along the tangential direction of the shell. Wherein the catalyst mother liquor refers to liquid returned to the reaction kettle from the bottom of the flash tank. Under the conditions of the reaction pressure of 2.8MPa and the temperature of 190 ℃, methanol and CO which are introduced into a reaction kettle react under the action of a catalyst to generate acetic acid, and a small amount of byproduct methyl acetate is generated.
The upper and lower two CO gas opposite spraying are adopted, the gas is sprayed from the center to the periphery through impact dispersion, and meanwhile, due to the phase difference pi between the upper and lower CO gas opposite spraying, when the flow of the upper air inlet is maximum, the flow of the lower air inlet is minimum. When the lower inlet flow is minimum, the upper inlet flow is maximum. The two gases are changed to cause the splashing gas to swing up and down, so that a large number of small bubbles are generated in the mixed solution, and the CO gas is uniformly distributed in the whole reaction kettle. The mixed liquid is introduced from two sides, flows in a vortex manner under the action of the cyclone, moves tangentially with small bubbles, and the bubbles are sheared to form smaller bubbles, so that the gas-liquid mass transfer process is facilitated, and the reaction rate is improved. The mixed liquid is stirred by the top methanol liquid jet flow, so that CO gas is uniformly distributed, and simultaneously, the sinking methanol liquid and the ascending CO gas move up and down mutually and are uniformly mixed, and the improvement of the reaction rate is facilitated.
As a specific implementation method, the CO flow control manner of the first nozzle 11 and the second nozzle 12 is a sine function.
As a specific implementation method, the liquid inlet 3 is positioned at 1/2-1/3 of the barrel from the bottom; the radial thickness of the cyclone 2 is 0.03-0.2 times of the diameter of the reaction kettle; the diameters of the nozzles at the upper CO inlet end part 11 and the lower CO inlet end part 12 are 0.01-0.1 times of the diameter of the reaction kettle; the nozzle spacing between the upper CO inlet end nozzle 11 and the lower CO inlet end nozzle 12 is 0.01-0.2 times of the diameter of the reaction kettle; the outlet of the nozzle 8 is positioned below the liquid level of the reaction kettle, and the height of the liquid level is preferably 0.1-0.5 times of the height of the liquid level below the liquid level; the CO flow rates at the outlets of the nozzle 11 and the nozzle 12 are changed at a certain frequency, and the phase difference pi exists between the two, preferably the change frequency is 2-20 Hz.
In a preferred embodiment, the top liquid inlet port nozzle 8 outlet flow rate is 8-25 m/s.
In a preferred embodiment, the CO inlet port nozzle 11 and nozzle 12 outlet flow rates are 8-25 m/s.
In a preferred embodiment, the liquid flow rate in the cyclone is 5-15 m/s.
Example 1
The oxo reactor shown in figure 1 is adopted, the height of the reaction kettle cylinder is 5m, the diameter is 3m, the diameter of the hemispherical head is 3m, and the liquid level of the reaction kettle is 5.5m. The diameter of the spinning machine (shown in fig. 2) was 2.4m, the diameter of the nozzle holes of the upper CO inlet end nozzle 11 and the lower CO inlet end nozzle 12 was 100mm, the nozzle hole spacing of the upper CO inlet end nozzle 11 and the lower CO inlet end nozzle 12 was 200mm, and the outlet of the nozzle 8 was located 1.2m below the liquid level of the reaction vessel. The CO flow at the outlets of the nozzle 11 and the nozzle 12 changes at a pulse frequency of 5Hz, and the two have a phase difference pi, and the outlet flow velocity of the two nozzles changes in the range of 8-15m/s; the top liquid inlet port nozzle 8 outlet flow rate is 8m/s; the methanol raw material liquid, the catalyst mother liquid and the dilute acid mixed liquid respectively enter the reactor from three liquid inlets 3 along the tangential direction of the shell, and flow in a vortex manner under the action of a cyclone, wherein the flow speed of the liquid in the cyclone is 10m/s. The circulating liquid flows out from the circulating liquid outlet 5, is cooled by the external circulating heat exchanger, enters the reaction kettle through the top liquid inlet 10, the CO gas raw material enters the reaction kettle through the upper CO inlet 6 and the lower CO inlet 7, and the reaction liquid is discharged from the reaction liquid outlet 4. Under the conditions of the reaction pressure of 2.8MPa and the temperature of 190 ℃, methanol and CO generate acetic acid in a catalyst system, and a small amount of methyl acetate is generated, and the operation result shows that the reaction kettle operates stably, the temperature fluctuation at the bottom of the reaction kettle is within 2 ℃, and the content of the byproduct methyl acetate is 0.52%.
Comparative example 1
At the same temperature, pressure and catalytic system as in example 1, the only difference from example 1 is that the CO all enters the reactor from nozzle 12; the methanol raw material liquid, the catalyst mother liquid and the dilute acid mixed liquid respectively enter the reactor directly from three liquid inlets 3 along the tangential direction of the shell. The operation result shows that the operation fluctuation of the reaction kettle is larger, the temperature fluctuation of the bottom of the reaction kettle is within 8-10 ℃, and the content of the byproduct methyl acetate is 1.54%.
Example 2
At the same temperature, pressure and catalytic system as in example 1, the only difference from example 1 is that the spacing between the upper CO inlet end nozzle 11 and the lower CO inlet end nozzle 12 is 500mm. The operation result shows that the reaction kettle operates stably, the temperature fluctuation at the bottom of the reaction kettle is within 4 ℃, and the content of the byproduct methyl acetate is 0.78%.
Example 3
At the same temperature, pressure and catalytic system as in example 1, the only difference from example 1 is that the CO flow at the outlet of nozzles 11 and 12 is varied at a pulse rate of 10Hz, and the top liquid inlet port nozzle 8 outlet flow rate is 12m/s. The operation result shows that the reaction kettle operates stably, the temperature fluctuation at the bottom of the reaction kettle is within 1 ℃, and the content of the byproduct methyl acetate is 0.42%.
The foregoing description of the preferred embodiments of the present invention is not intended to limit the invention, but any modifications, equivalents, improvements and modifications falling within the spirit and principles of the invention are intended to be included within the scope of the invention, and the technical content claimed in the present invention is fully set forth in the claims.
Claims (4)
1. A oxo process based on a oxo reactor comprising a reactor shell (1), at least one liquid inlet (3) tangential to the shell, a cyclone (2), a top liquid inlet (10), a recycle liquid outlet (5), a reaction liquid outlet (4), a gas outlet (9), two CO inlets; the ends of the two CO inlets, which are positioned in the reactor shell (1), are respectively provided with a first nozzle (11) and a second nozzle (12); the outlets of the first nozzle (11) and the second nozzle (12) are arranged in opposite directions and are positioned on the same vertical line;
the CO flow at the outlets of the first nozzle (11) and the second nozzle (12) is periodically changed at a certain pulse frequency, and a phase difference pi exists between the two; the end of the top liquid inlet (10) positioned in the reactor shell (1) is provided with a third nozzle (8); the outlets of the first nozzle (11) and the third nozzle (8) are vertically downward, and the outlet of the second nozzle (12) is vertically upward;
-the liquid inlet (3) tangential to the housing is arranged at a height between the first nozzle (11) and the second nozzle (12); the number of the liquid inlets (3) tangential to the shell is 3, the liquid inlets (3) tangential to the shell are positioned at the same height of the reactor shell, and the number of the liquid inlets (3) tangential to the shell are 120 degrees in the circumferential direction; a spinning jack (2) is arranged on the liquid inlet (3) tangential to the shell;
the distance between the first nozzle (11) and the second nozzle (12) is 0.01-0.2 times of the diameter of the reaction kettle;
the method is characterized in that the oxo synthesis method comprises the following steps:
CO gas enters the reactor from two CO inlets and is sprayed at a first nozzle (11) and a second nozzle (12); the CO flow at the outlets of the first nozzle (11) and the second nozzle (12) is periodically changed at a certain pulse frequency, and the two have a phase difference pi, so that the splashed CO gas swings up and down due to the change of the flow of the first nozzle (11) and the second nozzle (12), a large number of CO small bubbles are generated, and the CO gas is promoted to be uniformly distributed in the whole reaction kettle;
the methanol, the catalyst mother liquor and the dilute acid mixed liquor enter the reactor along the tangential direction of the shell through three liquid inlets (3) tangential to the shell; the gas flows in a vortex manner under the action of the cyclone (2), moves tangentially with CO small bubbles, and the bubbles are sheared to form smaller bubbles, so that the gas-liquid mass transfer process is facilitated;
the mixed liquid is stirred by the top methanol liquid jet flow, so that CO gas is uniformly distributed, and simultaneously, the sinking methanol liquid and the ascending CO gas move up and down mutually and are uniformly mixed, and the improvement of the reaction rate is facilitated.
2. The oxo process according to claim 1, wherein the outlet of the third nozzle (8) is located at a level of 0.1 to 0.5 times below the liquid level.
3. The oxo process according to claim 1, wherein the 3 liquid inlets (3) tangential to the shell are methanol inlet, catalyst mother liquor inlet and dilute acid mixed liquor inlet, respectively.
4. The oxo process according to claim 1, wherein the reactor shell (1) consists of a reactor vessel and upper and lower hemispherical/ellipsoidal heads.
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| JP2006022044A (en) * | 2004-07-08 | 2006-01-26 | Chiyoda Corp | Method for producing acetic acid with bubble tower type reactor |
| CN203196620U (en) * | 2013-04-24 | 2013-09-18 | 成都天成碳一化工有限公司 | Reactor for producing methyl formate through carbonylation |
| CN109134233A (en) * | 2018-10-19 | 2019-01-04 | 兖矿鲁南化工有限公司 | A kind of process units and production method of synthesizing acetic acid by methanol low-voltage carbonylation |
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| DE2553931B2 (en) * | 1975-12-01 | 1980-12-04 | Dynamit Nobel Ag, 5210 Troisdorf | Process and apparatus for the production of carboxylic acid esters or salts |
| US6362367B2 (en) * | 1998-04-21 | 2002-03-26 | Union Carbide Chemicals & Plastics Technology Corp. | Preparation of organic acids |
| WO2010105266A2 (en) * | 2009-03-13 | 2010-09-16 | University Of Utah Research Foundation | Fluid-sparged helical channel reactor and associated methods |
| CN104250208A (en) * | 2013-06-28 | 2014-12-31 | 中国石油化工股份有限公司 | Production method for preparing acetic acid through carbonylation of methanol |
| CN104941521A (en) * | 2014-03-31 | 2015-09-30 | 英尼奥斯欧洲股份公司 | Feeding distributor designed for ammonia oxidation reactor |
| CN206996240U (en) * | 2017-05-04 | 2018-02-13 | 绍兴鑫泓环保科技有限公司 | A kind of vortex pulse type reactor |
| CN114452903A (en) * | 2022-01-27 | 2022-05-10 | 中石化南京工程有限公司 | Oxo gas-liquid reactor |
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| JP2006022044A (en) * | 2004-07-08 | 2006-01-26 | Chiyoda Corp | Method for producing acetic acid with bubble tower type reactor |
| CN203196620U (en) * | 2013-04-24 | 2013-09-18 | 成都天成碳一化工有限公司 | Reactor for producing methyl formate through carbonylation |
| CN109134233A (en) * | 2018-10-19 | 2019-01-04 | 兖矿鲁南化工有限公司 | A kind of process units and production method of synthesizing acetic acid by methanol low-voltage carbonylation |
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