CN112844251A - Reaction device and system and method for synthesizing acetic acid by carbonyl - Google Patents
Reaction device and system and method for synthesizing acetic acid by carbonyl Download PDFInfo
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- CN112844251A CN112844251A CN202110014036.5A CN202110014036A CN112844251A CN 112844251 A CN112844251 A CN 112844251A CN 202110014036 A CN202110014036 A CN 202110014036A CN 112844251 A CN112844251 A CN 112844251A
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Abstract
The invention provides a reaction device, a system and a method for synthesizing acetic acid by carbonyl. The reaction device comprises a reaction kettle, a circulating fluid stirring part and a raw material gas distribution stirring part; the gas distribution stirring part comprises more than two gas distribution stirring units which are distributed in a multilayer way along the central shaft of the reaction kettle and are communicated; the circulating fluid feed pipe penetrates through the circulating fluid inlet and is communicated with the circulating fluid outlet; the raw material gas feeding pipe penetrates through the raw material gas inlet and is communicated with the gas distribution stirring part. The reaction device is adopted for carbonyl synthesis of acetic acid, so that the phenomenon that a shaft seal and a bottom fixed bearing are easy to damage in the operation process during mechanical stirring is avoided, no dynamic sealing point exists, and the safe and stable operation of a reaction system is guaranteed; meanwhile, the gas distribution stirring units which are distributed in a multilayer manner and are sequentially communicated enable the gas distribution in the reaction kettle to be more uniform, the gas-liquid two-phase mixing effect is improved, the reaction state in the system is optimized, the temperature difference in the reaction kettle is reduced, and the side reaction is reduced.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a reaction device, a system and a method for synthesizing acetic acid by carbonyl.
Background
Acetic acid is an important chemical intermediate and solvent for chemical reactions. The most common acetic acid synthesis process used at present is the methanol low-pressure carbonyl synthesis process, which is initiated in the 70 s by Monsanto company in America, and has made a major breakthrough in device productivity, product quality and production cost after decades of innovation and development. The conventional mechanical stirring mode is mostly adopted for gas-liquid stirring and mixing, and the liquid-liquid and gas-liquid mixing can be effectively carried out by adopting a reaction device for mechanical stirring, but a shaft seal and a bearing required by mechanical transmission are extremely easy to damage in long-term operation, so that the shutdown maintenance is caused, and the continuous, stable and safe operation is difficult to realize. In recent years, the hydraulic stirring is an important direction for improving the technology of the methanol oxo acetic acid synthesis device, and the hydraulic stirring technology mainly has the following problems: the single-layer ring distributor has gas distribution unevenness, thereby causing the catalyst to precipitate; the liquid is unevenly distributed, so that the reaction is uneven, and the temperature field is unevenly distributed; the production capacity is reduced, and the like.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a reaction device and a system and a method for synthesizing acetic acid by carbonyl, wherein the reaction device is adopted for producing the acetic acid by carbonyl synthesis, so that the phenomenon that a shaft seal and a bottom fixed bearing are easily damaged in the operation process during mechanical stirring is avoided, no dynamic sealing point exists in the whole reaction device, and the safe and stable operation of a reaction system is ensured; meanwhile, the gas distribution stirring units which are distributed in a multilayer manner and are sequentially communicated enable the gas distribution in the reaction kettle to be more uniform than that of the existing single-layer distributor, the gas-liquid two-phase mixing effect is improved, the reaction rate is increased, and the internal reaction state of the system is optimized.
The invention is realized by the following technical scheme:
the first aspect of the present invention provides a reaction apparatus comprising a reaction vessel, a circulating fluid stirring member and a raw material gas distribution stirring member; the reaction kettle comprises a raw material gas feeding pipe and is provided with a raw material gas inlet, a circulating fluid outlet and more than two circulating fluid inlets; the circulating fluid stirring part comprises more than two circulating fluid feeding pipes; the gas distribution stirring component is arranged in the reaction kettle and comprises more than two gas distribution stirring units which are distributed in a multilayer way along the central shaft of the reaction kettle and are communicated; the circulating fluid feed pipe penetrates through the circulating fluid inlet and is communicated with the circulating fluid outlet; the raw material gas feeding pipe penetrates through the raw material gas inlet and is communicated with the gas distribution stirring component.
Preferably, the included angle of the perpendicular projection of the central axes of the adjacent circulating fluid feed pipes on the radial plane of the reaction kettle is 60-150 degrees, such as 60-120 degrees or 120-150 degrees.
Preferably, each gas distribution stirring unit is annular and is respectively arranged along the central shaft of the reaction kettle; from a bottom layer gas distribution stirring unit close to the raw material gas inlet end to a top layer gas distribution stirring unit far away from the raw material gas inlet end, the diameters of all layers of gas distribution stirring units are sequentially increased, and the diameter calculation formula of the gas distribution stirring units is as follows:
Dni＝D*ni/(n+1)；
wherein D is the diameter of the reaction kettle, DniIs n thiThe outer circle diameter of the layer gas distribution stirring unit; n isi1, the gas distribution stirring unit is closest to the raw material gas inlet end; n isiThe number of layers counted from the gas distribution stirring unit closest to the raw material gas inlet end; n is the total number of layers of the gas distribution stirring member.
More preferably, at least one of the following technical characteristics is also included:
1) the sum of the distances between the adjacent gas distribution stirring units and the distance between the bottom layer gas distribution stirring unit and the bottom of the reaction kettle are less than or equal to the radius of the reaction kettle;
2) and the gas distribution stirring units of all layers are sequentially communicated from the bottom layer gas distribution stirring unit close to the raw material gas inlet end to the top layer gas distribution stirring unit far away from the raw material gas inlet end.
The sum of the heights of the adjacent gas distribution stirring units is less than or equal to the diameter of the reaction kettle.
Preferably, at least one of the following technical features is also included:
1) the gas distribution stirring unit is provided with gas holes which are uniformly and symmetrically or alternatively distributed;
2) the reaction kettle is also provided with a reaction liquid outlet for outputting reaction liquid;
3) a spray head is arranged at the end part of the circulating fluid feeding pipe arranged in the reaction kettle;
4) the raw material gas inlet is arranged at the bottom of the reaction kettle;
5) the circulating fluid outlet is arranged in the middle of the reaction kettle;
6) the circulating fluid inlet is arranged at the top of the reaction kettle;
7) the circulating fluid stirring part also comprises a circulating fluid pump and/or a circulating fluid heat exchanger, and the circulating fluid outlet is respectively connected with the more than two circulating fluid feeding pipes in more than two paths through the circulating fluid pump and/or the circulating fluid heat exchanger;
8) the raw material gas distribution stirring part is arranged at the bottom of the reaction kettle.
More preferably, at least one of the following technical characteristics is also included:
11) the characteristic 1) is that the diameter of the air hole is 2 mm-10 mm, such as 2 mm-6 mm, 6 mm-7 mm or 7 mm-10 mm;
12) the characteristic 1) is that the air hole distance is 20 mm-60 mm;
31) in the characteristic 3), the spray head is positioned in the middle of the reaction kettle;
32) in the characteristic 3), the spray head is of a reducing structure;
33) in the characteristic 3), the spray head is positioned below the liquid level of the reaction device at 1/6H-1/2H, such as 1/6H-2/6H, 2/6H-2/5H and 2/5H-1/2H, wherein H is the straight edge length of the cylinder of the reaction kettle;
71) in the characteristic 7), the circulating fluid stirring part comprises more than two circulating fluid pumps and/or more than two circulating fluid heat exchangers, the circulating fluid outlet is divided into more than two passages which are respectively connected with the more than two circulating fluid feeding pipes, and each passage is provided with one circulating fluid pump and/or one circulating fluid heat exchanger.
The invention provides a system for synthesizing acetic acid by carbonyl, which comprises the reaction device, a flash separator and a refining unit which are communicated in sequence.
Preferably, the flash separator is provided with a gas phase outlet and a liquid phase outlet, the gas phase outlet is communicated with the refining unit, and the liquid phase outlet is communicated with the reaction device.
The third aspect of the invention provides a method for synthesizing acetic acid by carbonyl, which adopts the reaction device, introduces reaction raw materials comprising methanol, CO and catalyst into the reaction device, adopts the circulating fluid stirring component and the gas distribution stirring component to stir materials, and generates acetic acid by reaction under the action of the catalyst.
Preferably, at least one of the following technical features is also included:
1) also comprises the following steps: carrying out flash separation on the reaction liquid to respectively obtain a gas-phase material and a liquid-phase material; refining the gas-phase material to obtain an acetic acid product, and refluxing the liquid-phase material to the reaction device;
2) the flow velocity of the air hole outlet of the gas distribution stirring unit is 5 m/s-30 m/s, such as 5 m/s-15 m/s, 15 m/s-20 m/s or 20 m/s-30 m/s;
3) the flow velocity of the fluid sprayed by the spray head of the circulating fluid feeding pipe is 5 m/s-20 m/s, such as 5 m/s-11 m/s, 11 m/s-15 m/s or 15 m/s-20 m/s; circulating fluid is sprayed out from a spray head at the end part of a circulating fluid feeding pipe at a high speed to drive peripheral liquid to change vectors, and the peripheral liquid turns upwards from the bottom of the reaction kettle to generate larger disturbance on the liquid in the reaction kettle, so that a plurality of large circulating flow states are formed in the reaction kettle, the liquid in the whole reaction kettle is ensured to be uniformly mixed, and the uniform distribution of the concentration field and the uniform distribution of the temperature field of the liquid in the reaction kettle are realized;
4) the total fluid flow of the outlets of more than two circulating fluid feeding pipes per hour is 5-10 times of the volume of the reaction liquid, such as 5-6.2 times, 6.2-7.5 times or 7.5-10 times.
The invention has the beneficial effects that:
the reaction device comprises a circulating fluid stirring part and a raw material gas distribution stirring part, is used for producing the acetic acid by the low-pressure carbonylation of the methanol, has no dynamic sealing point in the whole reaction device, eliminates the potential shutdown hazard possibly caused by the leakage of a mechanical seal during the mechanical stirring and the replacement required for the failure of the stirring part in a kettle caused by corrosion, ensures the safe and stable operation of the reaction system, and saves the expenditure of investment, operation and maintenance cost; the three-dimensional multilayer annular raw material gas distribution stirring component enables gas in the reaction kettle to be distributed more uniformly, improves the gas-liquid two-phase mixing effect, optimizes the reaction state in the system, reduces the temperature difference in the reaction kettle and reduces side reactions; the fluid circulation mixing system of configuration makes liquid distribution more even, and the temperature field is more even in the reation kettle, guarantees that production is more stable, and the productivity is promoted.
Drawings
FIG. 1 is a first schematic structural diagram of a reaction apparatus according to the present invention.
FIG. 2 is a schematic structural diagram II of the reaction apparatus of the present invention.
FIG. 3 is a schematic top view of two circulating fluid feeding pipes in the circulating fluid stirring part of the present invention.
FIG. 4 is a schematic top view of the gas distribution stirring member of the present invention.
FIG. 5 is a diagram of a system for oxo-synthesis of acetic acid.
Reference numerals
1 reaction apparatus
11 reaction kettle
1111 raw gas feeding pipe
1112 raw gas inlet
1121 circulating fluid outlet
1122 circulating fluid inlet
12 circulating fluid agitating member
121 circulating fluid feed pipe
1211 spray head
122 cycle fluid pump
123 circulating fluid heat exchanger
13 raw material gas distribution stirring member
131 gas distribution stirring unit
1311 air hole
2 flash separator
21 gas phase outlet
22 liquid phase outlet
3 refining unit
Detailed Description
The technical solution of the present invention is illustrated by specific examples below. It is to be understood that one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between the explicitly mentioned steps; it should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
A reaction apparatus, as shown in FIG. 1 and FIG. 2, comprises a reaction vessel 11, a circulating fluid stirring part 12 and a raw material gas distribution stirring part 13; the reaction kettle 11 comprises a raw material gas feeding pipe 1111, and the reaction kettle 11 is provided with a raw material gas inlet 1112, a circulating fluid outlet 1121 and more than two circulating fluid inlets 1122; the circulating fluid agitating unit 12 includes two or more circulating fluid feeding pipes 121; the gas distribution stirring part 13 is arranged in the reaction kettle 11, the gas distribution stirring part 13 comprises more than two gas distribution stirring units 131, and the more than two gas distribution stirring units are distributed in a multilayer manner along the central shaft of the reaction kettle and are communicated with each other; the circulating fluid feed line 121 extends through the circulating fluid inlet 1122 and communicates with the circulating fluid outlet 1121; the raw gas feed pipe 1111 penetrates the raw gas inlet 1112 and communicates with the gas distribution stirring section 13.
The three-dimensional multilayer gas distribution stirring component is used, so that the CO gas is uniformly distributed on the cross section of the reaction kettle and moves upwards after coming out of the gas holes with different heights, the CO bubble coalescence phenomenon is reduced, the CO gas in the whole reaction kettle exists in a smaller bubble form, the diffusion resistance of the CO to liquid is reduced, the gas distribution in the reaction kettle is ensured to be more uniform, and the gas-liquid two-phase mixing effect is improved.
In a preferred embodiment, the included angle of the perpendicular projection of the central axis of the adjacent circulating fluid feed pipes 121 on the radial plane of the reaction vessel is 60 ° to 150 °, which is α in fig. 3. This design ensures that liquid homogeneity is better in the reation kettle, and the reaction is more even in the reation kettle, and the difference in temperature reduces, and side reaction reduces.
In a preferred embodiment, as shown in fig. 1 and 4, each gas distribution stirring unit 131 is annular, each along the central axis of the reaction vessel; the diameters of the gas distribution stirring units 131 of each layer are sequentially increased from the bottom layer gas distribution stirring unit near the raw material gas inlet end to the top layer gas distribution stirring unit far from the raw material gas inlet end, and the diameter calculation formula of the gas distribution stirring units 131 is as follows:
Dni＝D*ni/(n+1)；
wherein D is the diameter of the reaction kettle, DniIs n thiThe outer circle diameter of the layer gas distribution stirring unit; n isi1, the gas distribution stirring unit is closest to the raw material gas inlet end; n isiThe number of layers counted from the gas distribution stirring unit closest to the raw material gas inlet end; n is the total number of layers of the gas distribution stirring member. The design ensures that the gas is uniformly distributed, the reaction in the reaction kettle is relatively uniform, the temperature difference is reduced, and the side reaction is reduced.
As shown in fig. 1 and fig. 4, the gas distribution stirring component 13 is a multilayer annular pipe body interconnection structure, the outer circle diameter D1 of the first layer of annular, the outer circle diameter D2 of the second layer of annular, and the outer circle diameter D3 of the third layer of annular sequentially increase to Dn, D1 is D1/(n +1), D2 is D2/(n +1), and so on, where D is the diameter of the reaction kettle, and n is the total number of layers of the gas distribution stirring component.
In a preferred embodiment, the sum of the distances between the adjacent gas distribution stirring units and the distance between the bottom layer gas distribution stirring unit and the bottom of the reaction kettle is less than or equal to the radius of the reaction kettle. For example: the height between the bottom of the reaction kettle and a bottom layer gas distribution stirring unit, namely the height between the first layer of circular rings, is H1, the height between the bottom layer gas distribution stirring unit, namely the height between the first layer of circular rings and the second layer of circular rings, is H2, the height between the second layer of circular rings and the third layer of circular rings is H3, the height between the n-1 th layer of circular rings and the n-th layer of circular rings is Hn in turn, and H1+ H2+ H3+ … Hn is less than or equal to the radius of the reaction kettle. The design ensures that the gas is uniformly distributed, the reaction in the reaction kettle is relatively uniform, the temperature difference is reduced, and the side reaction is reduced.
In a preferred embodiment, the gas distribution stirring units 131 of each layer are sequentially communicated from the bottom layer gas distribution stirring unit near the raw material gas inlet end to the top layer gas distribution stirring unit far from the raw material gas inlet end.
In a preferred embodiment, the gas distribution stirring unit 131 is provided with uniformly symmetrical or staggered gas holes 1311.
In a preferred embodiment, the diameter of the air holes is 2mm to 10 mm.
In a preferred embodiment, the air hole pitch is 20mm to 60 mm.
In a preferred embodiment, the reaction vessel 11 is further provided with a reaction liquid outlet for outputting the reaction liquid.
In a preferred embodiment, a spray nozzle 1211 is disposed at the end of the circulating fluid feed pipe 121 disposed in the reaction vessel 11.
In a preferred embodiment, the nozzle 1211 is located in the middle of the reaction vessel 11.
In a preferred embodiment, the nozzle 1211 is a reduced diameter structure. The design can ensure that the liquid at the outlet of the spray head is sprayed out at a higher speed.
In a preferred embodiment, the nozzle 1211 is located below the liquid level of the reaction device from 1/6H to 1/2H, wherein H is the straight-edge length of the cylinder of the reaction kettle. This design makes liquid mixture more even, and the reaction is more even among the reation kettle, and the difference in temperature reduces, and side reaction reduces.
In a preferred embodiment, the feed gas inlet 1112 is provided at the bottom of the reaction vessel 11.
In a preferred embodiment, the circulating fluid outlet 1121 is provided at the middle of the reaction tank 11.
In a preferred embodiment, the circulating fluid inlet 1122 is provided at the top of the reaction vessel 11.
In a preferred embodiment, the circulating fluid stirring part 12 further comprises a circulating fluid pump 122 and/or a circulating fluid heat exchanger 123, and the circulating fluid outlet 1121 is connected to the two or more circulating fluid feeding pipes 121 through two or more paths of the circulating fluid pump 122 and/or the circulating fluid heat exchanger 123, respectively. As shown in fig. 1, the circulating fluid outlet is connected to a circulating fluid pump 122, and after being cooled by a circulating fluid heat exchanger 123, the circulating fluid is divided into two parts which respectively enter the reaction kettle through two circulating fluid feeding pipes 121, and are ejected out from the nozzle at the end part at a high speed, so that the liquid in the reaction kettle is uniformly stirred and mixed.
In a preferred embodiment, the circulating fluid stirring part 12 includes two or more circulating fluid pumps 122 and/or two or more circulating fluid heat exchangers 123, the circulating fluid outlet 1121 is divided into two or more paths to be respectively connected to the two or more circulating fluid feeding pipes 121, and each path is provided with one circulating fluid pump 122 and/or one circulating fluid heat exchanger 123. As shown in fig. 2, the circulating fluid outlet is divided into two parts, which are respectively connected to a circulating fluid pump 122, and after being cooled by a circulating fluid heat exchanger 123, the two parts enter the reaction kettle through two circulating fluid feeding pipes 121, and are sprayed out from the spray head at the end part at a high speed, so as to uniformly stir and mix the liquid in the reaction kettle.
In a preferred embodiment, the raw material gas distribution stirring part 13 is provided at the bottom of the reaction vessel 11.
More preferably, at least one of the following technical characteristics is also included:
the second aspect of the present invention provides a system for oxo-synthesis of acetic acid, as shown in fig. 5, comprising the above reaction apparatus 1, flash separator 2 and refining unit 3, which are connected in sequence.
In a preferred embodiment, the flash separator 2 is provided with a gas phase outlet 21 and a liquid phase outlet 22, the gas phase outlet 21 being in communication with the refining unit 3 and the liquid phase outlet 22 being in communication with the reaction device 1.
The following examples 1 to 3 employ a preferred reaction apparatus, as shown in FIGS. 1, 3 and 4, comprising a reaction vessel 11, a circulating fluid stirring section 12 and a raw material gas distribution stirring section 13; the reaction kettle 11 comprises a raw material gas feeding pipe 1111, and the reaction kettle 11 is provided with a raw material gas inlet 1112, a circulating fluid outlet 1121 and more than two circulating fluid inlets 1122; the circulating fluid agitating unit 12 includes two or more circulating fluid feeding pipes 121; the gas distribution stirring part 13 is arranged in the reaction kettle 11, the gas distribution stirring part 13 comprises more than two gas distribution stirring units 131, and the more than two gas distribution stirring units are distributed in a multilayer manner along the central shaft of the reaction kettle and are communicated with each other; the circulating fluid feed line 121 extends through the circulating fluid inlet 1122 and communicates with the circulating fluid outlet 1121; the raw gas feed pipe 1111 penetrates the raw gas inlet 1112 and communicates with the gas distribution stirring section 13. Each gas distribution stirring unit 131 is annular and is respectively arranged along the central shaft of the reaction kettle; the diameters of the gas distribution stirring units 131 of each layer are sequentially increased from the bottom layer gas distribution stirring unit near the raw material gas inlet end to the top layer gas distribution stirring unit far from the raw material gas inlet end, and the diameter calculation formula of the gas distribution stirring units 131 is as follows:
Dni＝D*ni/(n+1)；
wherein D is the diameter of the reaction kettle, DniIs n thiThe outer circle diameter of the layer gas distribution stirring unit; n isi1, the gas distribution stirring unit is closest to the raw material gas inlet end; n isiThe number of layers counted from the gas distribution stirring unit closest to the raw material gas inlet end; n is the total number of layers of the gas distribution stirring member. The gas distribution stirring units 131 of each layer are sequentially communicated from the bottom layer gas distribution stirring unit near the raw material gas inlet end to the top layer gas distribution stirring unit far from the raw material gas inlet end. The reaction kettle 11 is also provided with a reaction liquid outlet for outputting reaction liquid. A spray nozzle 1211 is disposed at the end of the circulating fluid feeding pipe 121 disposed in the reaction kettle 11. The nozzle 1211 is located in the middle of the reaction kettle 11. The nozzle 1211 has a diameter-reducing structure. The nozzle 1211 is positioned below the liquid level of the reaction device at 1/6H-1/2H, wherein H is the straight edge length of the cylinder of the reaction kettle. The raw material gas inlet 1112 is provided at the bottom of the reaction vessel 11. The circulating fluid outlet1121 is arranged in the middle of the reaction kettle 11. The circulating fluid inlet 1122 is provided at the top of the reaction vessel 11. The circulating fluid stirring part 12 further comprises a circulating fluid pump 122 and a circulating fluid heat exchanger 123, and the circulating fluid outlet 1121 is connected to the two or more circulating fluid feeding pipes 121 through the circulating fluid pump 122 and the circulating fluid heat exchanger 123 in two or more paths respectively. The raw material gas distribution stirring part 13 is arranged at the bottom of the reaction kettle 11.
Comparative example
The industrial device for synthesizing acetic acid by methanol at low pressure adopts a mechanical stirring device before the transformation of a reaction kettle, the height of a barrel of the reaction kettle is 5m, the diameter of the barrel is 3m, a single-layer pipe body CO distributor is provided with an outer circle diameter of 2m, the CO distributor is provided with uniformly symmetrical air holes, the diameter of each air hole is 15mm, the diameter of each outer circle is 1m, and an outlet of a circulating fluid feeding pipe (one) is positioned above the liquid level and has no diameter reduction. Under certain temperature and pressure and in the presence of catalyst, methanol and CO produce carbonylation reaction to produce acetic acid, and the axial temperature difference in the reaction kettle is about 3 deg.c.
Example 1
A reaction device for synthesizing acetic acid by methanol under low pressure is characterized in that the height of a cylinder of a reaction kettle (namely the straight edge length of the cylinder of the reaction kettle) is 5m, the diameter of the cylinder is 3m, the reaction kettle is improved by adopting a circulating fluid stirring component and a three-dimensional multi-ring raw material gas distribution stirring component shown in figures 1, 3 and 4, the included angle of the vertical projection of the central axes of two circulating fluid feeding pipes on the radial plane of the reaction kettle is 150 degrees, the end spray heads of the two circulating fluid feeding pipes are positioned at 5/6m (which is 1/6 of the straight edge length of the cylinder of the reaction kettle) below the liquid level, the flow rate of fluid sprayed by the spray heads of the circulating fluid feeding pipes is 5m/s, and the total flow3The volume of the reaction solution is 5 times of the volume of the reaction solution. The raw material gas distribution stirring part comprises two gas distribution stirring units 131, namely two layers, the diameters of the outer circles are 1m and 2m respectively, uniformly symmetrical air holes are formed in the gas distribution stirring units, the diameters of the air holes are 6mm, the average air speed of the air outlet holes is 5m/s, and the sum of the distances between every two adjacent gas distribution stirring units and the distance between the bottom layer gas distribution stirring unit, namely the distance between the first layer gas distribution stirring unit and the bottom of the reaction kettle is 1.2 m. In comparison with the comparative exampleUnder the conditions of the same temperature and pressure and the existence of the catalyst, the methanol and the CO carry out carbonylation reaction to generate the acetic acid, the axial temperature of the reaction kettle is reduced by 2 ℃ compared with the comparative example, namely the axial temperature difference of the reaction kettle is about 1 ℃, and the propionic acid content in the product is reduced by 100 ppm.
Example 2
A reaction device for synthesizing acetic acid by methanol at low pressure is provided, the height of a barrel of a reaction kettle is 5m, the diameter of the barrel is 3m, the reaction kettle is improved by adopting a circulating fluid stirring part and a three-dimensional multi-ring raw gas distribution stirring part which are shown in figures 2, 3 and 4, 3 circulating fluid feeding pipes, the included angle of the vertical projection of the central axis of the adjacent circulating fluid feeding pipe 121 on the radial plane of the reaction kettle is 120 degrees, the end spray head of the circulating fluid feeding pipe is positioned at 10/6m below the liquid level (which is 2/6 of the straight edge length of the barrel of the reaction kettle), the flow rate of fluid sprayed out by the spray head of the circulating fluid feeding pipe is 11m/s, and the total flow rate of3The volume of the reaction solution was 6.2 times. The raw material gas distribution stirring part comprises three gas distribution stirring units 131, namely three layers, the diameters of the outer circles of the three gas distribution stirring units are respectively 0.75m, 1.5m and 2.25m, uniformly and symmetrically arranged gas holes are formed in the gas distribution stirring units, the diameters of the gas holes are 10mm, the average gas velocity of the gas outlet holes is 15m/s, and the sum of the distances between the adjacent gas distribution stirring units and the distance between the bottom layer gas distribution stirring unit, namely the distance between the first layer gas distribution stirring unit and the bottom of the reaction kettle is 1.0 m. Under the conditions of the same temperature and pressure as those of the comparative example and the existence of the catalyst, the methanol and the CO carry out carbonylation reaction to generate the acetic acid, the axial temperature of the reaction kettle is reduced by 1 ℃ compared with the comparative example, namely the axial temperature difference of the reaction kettle is about 2 ℃, and the content of the propionic acid in the product is reduced by 70 ppm.
Example 3
A reaction device for synthesizing acetic acid by methanol under low pressure is characterized in that the height of a reaction kettle barrel body is 5m, the diameter of the reaction kettle barrel body is 3m, after the reaction kettle is modified, a circulating fluid stirring part and a three-dimensional multi-ring raw material gas distribution stirring part which are shown in figures 2, 3 and 4 are adopted, four circulating fluid feeding pipes are adopted, the included angle of the vertical projection of the central shaft of the adjacent circulating fluid feeding pipe 121 on the radial plane of the reaction kettle is 60 degrees, and the end part spray head of each circulating fluid feeding pipe is positioned 15/6m below the liquid level (the length of the straight side of the1/2 degrees), the flow velocity of the fluid sprayed from the spray head of the circulating fluid feed pipe is 15m/s, and the total flow of the fluid at the outlet of the circulating fluid feed pipe is 320m3The volume of the reaction liquid is 7.5 times, the raw material gas distribution stirring part comprises four gas distribution stirring units 131, namely four layers, the diameters of the outer circles of the four gas distribution stirring units are respectively 0.6m, 1.2m, 1.8m and 2.4m, uniform and symmetrical air holes are formed in the gas distribution stirring units, the diameters of the air holes are 2mm, the average gas velocity of the air outlet holes is 20m/s, and the distance between the adjacent gas distribution stirring units plus the distance between the bottom layer gas distribution stirring unit, namely the distance between the first layer gas distribution stirring unit and the bottom of the reaction kettle is 1.2 m. Under the conditions of the same temperature and pressure as those of the comparative example and the existence of the catalyst, the methanol and the CO carry out carbonylation reaction to generate the acetic acid, the axial temperature of the reaction kettle is reduced by 0.5 ℃ compared with the comparative example, namely the axial temperature difference of the reaction kettle is about 2.5 ℃, and the content of the propionic acid in the product is reduced by 80 ppm.
Example 4
A reaction device for synthesizing acetic acid by methanol at low pressure is provided, the height of a reaction kettle barrel is 5m, the diameter is 3m, after the reaction kettle is transformed, a circulating fluid stirring part and a three-dimensional multi-ring raw material gas distribution stirring part which are shown in figures 2, 3 and 4 are adopted, the included angle of the vertical projection of the central axes of two circulating fluid feeding pipes on the radial plane of the reaction kettle is 120 degrees, the end nozzles of the two circulating fluid feeding pipes are positioned at 12/6 (which is 2/5 of the straight edge length of the barrel of the reaction kettle) below the liquid level, the flow rate of fluid sprayed out by the nozzles of the circulating fluid feeding pipes is 20m/s, and the total flow rate of fluid at the outlet of3The volume of the reaction liquid is 10 times, the raw material gas distribution stirring component comprises five gas distribution stirring units 131, namely five layers, the diameters of the outer circles of the five gas distribution stirring units are respectively 0.5m, 1m, 1.5m, 2m and 2.5m, uniform and symmetrical air holes are formed in the gas distribution stirring units, the diameters of the air holes are 7mm, the average gas velocity of the air outlet holes is 30m/s, the sum of the distances between the adjacent gas distribution stirring units and the bottom layer gas distribution stirring unit, namely the distance between the first layer gas distribution stirring unit and the bottom of the reaction kettle is 1.4 m. Under the conditions of same temperature and pressure as those of the comparative example and the existence of the catalyst, the methanol and the CO carry out carbonylation reaction to generate the acetic acid, and the axial temperature of the reaction kettle is reduced by 2.5 ℃ compared with the comparative example, namely the axial temperature difference of the reaction kettleAbout 0.5 ℃, and the content of propionic acid in the product is reduced by 120 ppm.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (10)
1. A reaction device is characterized by comprising a reaction kettle (11), a circulating fluid stirring part (12) and a raw material gas distribution stirring part (13); the reaction kettle (11) comprises a raw material gas feeding pipe (1111), and the reaction kettle (11) is provided with a raw material gas inlet (1112), a circulating fluid outlet (1121) and more than two circulating fluid inlets (1122); the circulating fluid stirring part (12) comprises more than two circulating fluid feeding pipes (121); the gas distribution stirring component (13) is arranged in the reaction kettle (11), the gas distribution stirring component (13) comprises more than two gas distribution stirring units (131), and the more than two gas distribution stirring units are distributed in a multilayer manner along the central shaft of the reaction kettle and are communicated with each other; the circulating fluid feed pipe (121) extends through the circulating fluid inlet (1122) and communicates with the circulating fluid outlet (1121); the raw gas feed pipe (1111) penetrates the raw gas inlet (1112) and communicates with the gas distribution stirring part (13).
2. The reactor according to claim 1, wherein the angle of the perpendicular projection of the central axes of adjacent circulating fluid feed pipes (121) on the radial plane of the reactor is 60 ° to 150 °.
3. The reaction device according to claim 1, wherein each gas distribution stirring unit (131) is annular and is arranged along the central axis of the reaction kettle; the diameters of the gas distribution stirring units (131) of each layer are sequentially increased from a bottom layer gas distribution stirring unit close to the raw material gas inlet end to a top layer gas distribution stirring unit far from the raw material gas inlet end, and the diameter calculation formula of the gas distribution stirring units (131) is as follows:
Dni＝D*ni/(n+1)；
wherein D is the diameter of the reaction kettle, DniIs n thiThe outer circle diameter of the layer gas distribution stirring unit; n isi1, the gas distribution stirring unit is closest to the raw material gas inlet end; n isiThe number of layers counted from the gas distribution stirring unit closest to the raw material gas inlet end; n is the total number of layers of the gas distribution stirring member.
4. The reactor device according to claim 3, characterized in that it further comprises at least one of the following technical features:
1) the sum of the distances between the adjacent gas distribution stirring units and the distance between the bottom layer gas distribution stirring unit and the bottom of the reaction kettle are less than or equal to the radius of the reaction kettle;
2) from the bottom layer gas distribution stirring unit close to the raw material gas inlet end to the top layer gas distribution stirring unit far away from the raw material gas inlet end, the gas distribution stirring units (131) of each layer are communicated in sequence.
5. The reactor device according to claim 1, characterized in that it further comprises at least one of the following technical features:
1) the gas distribution stirring unit (131) is provided with gas holes (1311) which are uniformly and symmetrically or alternatively distributed;
2) the reaction kettle (11) is also provided with a reaction liquid outlet for outputting reaction liquid;
3) a spray head (1211) is arranged at the end part of the circulating fluid feeding pipe (121) arranged in the reaction kettle (11);
4) the raw material gas inlet (1112) is arranged at the bottom of the reaction kettle (11);
5) the circulating fluid outlet (1121) is arranged in the middle of the reaction kettle (11);
6) the circulating fluid inlet (1122) is arranged at the top of the reaction kettle (11);
7) the circulating fluid stirring part (12) further comprises a circulating fluid pump (122) and/or a circulating fluid heat exchanger (123), and the circulating fluid outlet (1121) is respectively connected with the more than two circulating fluid feeding pipes (121) in more than two paths through the circulating fluid pump (122) and/or the circulating fluid heat exchanger (123);
8) the raw material gas distribution stirring part (13) is arranged at the bottom of the reaction kettle (11).
6. The reactor device according to claim 5, characterized in that it further comprises at least one of the following technical features:
11) characterized in that 1) the diameter of the air hole is 2 mm-10 mm;
12) the characteristic 1) is that the air hole distance is 20 mm-60 mm;
31) in the characteristic 3), the spray head (1211) is positioned in the middle of the reaction kettle (11);
32) in the characteristic 3), the spray head (1211) is of a reducing structure;
33) in the characteristic 3), the spray head (1211) is positioned below the liquid level of the reaction device at 1/6H-1/2H, wherein H is the straight-edge length of the cylinder of the reaction kettle;
71) in the characteristic 7), the circulating fluid stirring part (12) comprises more than two circulating fluid pumps (122) and/or more than two circulating fluid heat exchangers (123), the circulating fluid outlet (1121) is divided into more than two paths which are respectively connected with the more than two circulating fluid feeding pipes (121), and each path is provided with one circulating fluid pump (122) and/or one circulating fluid heat exchanger (123).
7. A system for oxo synthesis of acetic acid, comprising a reaction apparatus (1) according to any one of claims 1 to 6, a flash separator (2) and a refining unit (3) in sequential communication.
8. An oxo-acetic acid system according to claim 7, wherein the flash separator (2) is provided with a gas phase outlet (21) and a liquid phase outlet (22), the gas phase outlet (21) being in communication with the refining unit (3) and the liquid phase outlet (22) being in communication with the reaction apparatus (1).
9. A method for synthesizing acetic acid by carbonyl, characterized in that, the reaction device of any claim 1 to 6 is adopted, reaction raw materials comprising methanol, CO and catalyst are introduced into the reaction device, and the circulating fluid stirring component and the gas distribution stirring component are adopted to stir the materials, and the materials are reacted under the action of the catalyst to generate the acetic acid.
10. An oxo acetic acid according to claim 9, further comprising at least one of the following technical features:
1) also comprises the following steps: carrying out flash separation on the reaction liquid to respectively obtain a gas-phase material and a liquid-phase material; refining the gas-phase material to obtain an acetic acid product, and refluxing the liquid-phase material to the reaction device;
2) the flow velocity of the air hole outlet of the gas distribution stirring unit is 5-30 m/s;
3) the flow velocity of the fluid sprayed by the spray head of the circulating fluid feeding pipe is 5-20 m/s;
4) the total fluid flow of the outlets of more than two circulating fluid feed pipes per hour is 5-10 times of the volume of the reaction liquid.
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| CN202110014036.5A CN112844251A (en) | 2021-01-06 | 2021-01-06 | Reaction device and system and method for synthesizing acetic acid by carbonyl |
| PCT/CN2021/132466 WO2022148162A1 (en) | 2021-01-06 | 2021-11-23 | Reaction device, and system and method for synthesizing acetic acid from carbonyl |
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| CN202110014036.5A CN112844251A (en) | 2021-01-06 | 2021-01-06 | Reaction device and system and method for synthesizing acetic acid by carbonyl |
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| WO2022148162A1 (en) * | 2021-01-06 | 2022-07-14 | 上海华谊能源化工有限公司 | Reaction device, and system and method for synthesizing acetic acid from carbonyl |
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