CN108246222B - Long-shaft magnetic pump type reactor - Google Patents
Long-shaft magnetic pump type reactor Download PDFInfo
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- CN108246222B CN108246222B CN201810008798.2A CN201810008798A CN108246222B CN 108246222 B CN108246222 B CN 108246222B CN 201810008798 A CN201810008798 A CN 201810008798A CN 108246222 B CN108246222 B CN 108246222B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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Abstract
The invention relates to a novel long-shaft magnetic pump type reactor, which mainly solves the problem of uneven mixing of gas-liquid-solid three phases in the prior art. The invention adopts a novel long shaft magnetic pump type reactor, wherein 1-2 long shafts penetrate through the reactor, the long shaft is wrapped by a long sleeve, a bearing is additionally arranged in the reactor to completely isolate the shaft and the bearing from a medium on the outer side, a paddle soaked in the medium is coupled with the shaft by utilizing the principle of a magnetic pump to realize the stirring effect, each layer of tower plate in the reactor is provided with a riser, the air inlet of the riser is arranged on one side of the long shaft of the reactor, the upper part of the riser is connected with a gas distributor, the center of the gas distributor is positioned on the long shaft, gas phase from the lower layer of tower plate is uniformly sprayed into a liquid-solid mixture on the tower plate through the gas distributor, and each layer of tower plate is provided with a liquid phase inlet and outlet facility, so that the technical scheme better solves the problems and can be used in gas-liquid-solid three-phase catalytic reaction.
Description
Technical Field
The invention relates to a novel long-shaft magnetic pump type reactor.
Background
With the rise and development of green chemical industry, chemical process strengthening technology is more and more concerned. The reaction rectification technology which integrates chemical reaction and rectification separation to form a multifunctional reaction device is one of the ways for realizing the enhancement of the chemical process. The catalytic rectification is a heterogeneous catalytic rectification technology developed on the basis of homogeneous reactive rectification, and the technology places a solid catalyst on each layer of tower plate of a reaction section in a tower, gas and liquid respectively flow in a countercurrent manner upwards and downwards, chemical reaction and rectification separation are highly coupled in the tower, reaction products can be continuously removed, and the reaction heat can also be used as vaporization heat in the rectification process. Compared with a continuous stirred tank reactor connected in series, the catalytic rectifying tower has the advantages of low investment, low energy consumption, high conversion rate, high selectivity, high production capacity and the like, and is applied to chemical processes such as etherification, alkylation, ether hydrolysis, ester hydrolysis, esterification, ester exchange, dimerization, hydrogenation, isomerization, dehydration and the like. For gas-liquid-solid three-phase catalytic rectification of solid particles or particle catalysts, uniform mixing of gas-liquid-solid three phases among tower plates is a difficult point, and the design of a safe and reliable catalytic rectification tower suitable for continuous stirring and uniform mixing is very necessary.
Patent CN 101618304 a describes an esterification reactor, which can perform gas-liquid-solid three-phase continuous stirring on each layer of tower plate by connecting a rotatable gas distributor on the upper part of a riser, but is limited by the power brought by the gas flow rate, and the solid particle catalyst on each layer of tower plate can not ensure sufficient stirring and uniform mixing.
Patent CN 1015175211A proposes that high-purity isobutene prepared by dehydration of tertiary butanol is subjected to catalytic rectification by using a windowing flow guide type structured packing, the method is simple, the effect is good, but the catalyst is difficult to replace, and the catalyst is required to have a longer service life.
Patent CN 105561911A proposes a catalyst bundling filler in a high-efficiency catalytic rectification tower and a preparation method thereof, solid catalyst particles are filled in a catalyst package, and a catalyst package chain and a regular corrugated filler sheet are tightly attached to each other and coiled and then are fixedly formed by a tightening sheet. The hollow structure of the catalyst bag increases the gas-liquid mass transfer space, can effectively promote the reaction, but the catalyst is difficult to replace, and can be replaced only by stopping the vehicle, so that the requirement on the service life of the catalyst is high.
Patent CN101219950A provides a system and a method for preparing n-butyl acetate by using transesterification of methyl acetate and n-butanol, the catalytic rectification tower is composed of a stripping section, a reaction section and a rectification section, wherein the reaction section is composed of a liquid collecting plate, a gas rising pipe, a catalyst bag, a supporting plate and a bottom plate, the operation is simple, the conversion rate of methyl acetate is high, but the catalyst bag is difficult to replace.
Patent CN 205731266 discloses a kettle-type agitator, adopts two helical ribbon helical structure's stirring blade, and the stirring is more thorough, has improved stirring efficiency and effect, but stirring rake bearing and transmission shaft often can suffer rapidly and corrode, lead to frequently overhauing, increase the maintenance cost.
Disclosure of Invention
The invention aims to solve the technical problem of uneven gas-liquid-solid three-phase mixing in the prior art and provides a novel long-shaft magnetic pump type reactor. The reactor has the advantage of uniform mixing of gas, liquid and solid phases.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a novel long shaft magnetic pump type reactor is characterized in that 1-2 long shafts penetrate through the reactor, the long shafts are wrapped by long sleeves, bearings are additionally arranged inside the reactor to completely isolate the shafts and the bearings from media outside, blades soaked in the media are coupled with the shafts by utilizing the principle of a magnetic pump to realize the stirring effect, a riser is arranged on each layer of tower plate in the reactor, an air inlet of the riser is arranged on one side of the long shaft of the reactor, and the upper part of the riser is connected with a gas distributor, the center of the gas distributor is positioned on the long shaft, the gas phase from the lower tower plate is uniformly sprayed into the liquid-solid mixture on the tower plate through the gas distributor, each layer of tower plate is provided with a liquid phase inlet and outlet facility, liquid phase feed inlets and liquid phase outlets are respectively arranged on two sides of the tower plate, liquid phase of the tower plate enters the lower tower plate outside the tower, or a downcomer is arranged on the tower plate, and liquid phase in the tower flows to the lower tower plate from the upper tower plate; the solid particle or particle catalyst is placed on each layer of tower plate, and each layer of tower plate of the reactor is provided with a catalyst loading and unloading opening, so that the catalyst can be replaced without stopping the reactor; wherein the distance between two adjacent tower plates is H, the inner diameter of the tower is D, and the range of H is 300-700 mm; the diameter range of the holes of the outer pipe of the gas distributor is 2-25 mm, the diameter range of the holes of the inner pipe is 1-20 mm, and the holes are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.05-0.25, the distance between the center of the inlet of the riser and the center of the tower plate is 0.1-0.3D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.08-0.25, the distance between the central line of the downcomer and the center of the tower plate is 0.20-0.45D, the downcomer needs to extend below the liquid level of the tower plate, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.4-0.9.
In the above technical scheme, preferably, a filter screen is arranged at the liquid phase outlet or the downcomer inlet to prevent the catalyst from entering the lower-layer tower plate.
In the above technical solution, preferably, the gas distributor is a ring gas distributor.
In the above technical solution, more preferably, the gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the tower inner diameter D is 0.3 to 0.8, the ratio of the inner pipe diameter b to the tower inner diameter D is 0.2 to 0.7, and the center of the double-ring gas distributor coincides with the center of the tower plate.
In the technical scheme, preferably, the distance between two adjacent tower plates is H, the inner diameter of the tower is D, and the range of H is 400-600 mm; the diameter range of the holes of the outer pipe of the gas distributor is 5-20 mm, the diameter range of the holes of the inner pipe is 5-15 mm, and the holes are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.1-0.15; the distance between the center of the riser inlet and the center of the tower plate is 0.1-0.2D; the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.1-0.15; the distance between the central line of the downcomer and the center of the tower plate is 0.3-0.4D; the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.6-0.8.
In the above technical solution, preferably, a magnetic pump type stirrer is provided in the reactor.
In the above technical solution, preferably, the medium is a gas-liquid-solid three phase.
The invention provides a novel long-shaft magnetic pump type reactor, aiming at solving the problem of uneven mixing of gas, liquid and solid phases between plates in the existing catalytic distillation tower. The reactor has the characteristics of good gas-liquid-solid three-phase mixing effect, isolation shaft and bearing, reliable magnetic stirring operation and the like; the solid particle or particle catalyst is placed on each layer of tower plate, and because the density of the solid is close to that of the liquid, the solid catalyst is suspended and dispersed in the liquid phase under the action of the stirring paddle, so that gas, liquid and solid phases in the reaction device are fully stirred and uniformly mixed, and the reaction efficiency is good. Meanwhile, each layer of tower plate of the reactor is provided with a catalyst loading and unloading opening, so that the catalyst can be replaced without stopping. The invention has the characteristics of continuous stirring, uniform mixing of gas, liquid and solid phases, safe and reliable structure, stable operation and the like, and obtains better technical effect.
Drawings
FIG. 1 is a schematic diagram of the reactor of the present invention, illustrating only the structure of two adjacent trays at the top of the column.
In fig. 1, a magnetic stirrer 1, a long shaft 3, a long shaft sleeve 4, a paddle 4, a heavy component feed port 5, a gas distributor 7, a riser 8, a liquid phase inlet 9, a catalyst replenishing port 10, a tower body 12, a filter screen 13, a liquid phase outlet 14, a tower plate 15, a catalyst outlet 16.
FIG. 2 is a second schematic diagram of the reactor of the present invention, illustrating only the structure of two adjacent trays at the top of the column.
In fig. 2, a magnetic stirrer 1, a long shaft 3, a long shaft sleeve 4, a paddle 4, a blade 5, a heavy component feeding port 6, a gas distributor 7, a riser 8, a tower body 9, a catalyst replenishing port 10, a tower plate 11, a filter screen 12, a tower plate 13, a downcomer 14 and a catalyst outlet are arranged.
FIG. 3 is a schematic flow chart of the rectification process for preparing butyl acetate by the transesterification of methyl acetate and n-butanol in the example.
In fig. 3, 1 a catalytic distillation column 2, a condenser 3, a reflux tank 4, a reboiler 5, and a reflux pump.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
A novel long shaft magnetic pump type reactor is disclosed, as shown in figure 1, the reactor is internally penetrated by 1 long shaft, the long shaft is wrapped by a long sleeve, a bearing is additionally arranged in the reactor to completely isolate the shaft and the bearing from a medium on the outer side, a paddle soaked in the medium is coupled with the shaft by utilizing the principle of a magnetic pump to realize the stirring effect, each layer of tower plate in the reactor is provided with a riser, the air inlet of the riser is arranged on one side of the long shaft of the reactor, the upper part of the riser is connected with a gas distributor, the center of the gas distributor is arranged on the long shaft, gas phase from a lower layer of tower plate is uniformly sprayed into a liquid-solid mixture on the tower plate through the gas distributor, each layer of tower plate is provided with a liquid phase inlet and outlet facility, both sides of the tower plate are respectively provided with a liquid phase inlet and a liquid phase outlet; the solid particle or particle catalyst is placed on each layer of tower plate, and each layer of tower plate of the reactor is provided with a catalyst loading and unloading opening, so that the catalyst can be replaced without stopping the reactor; wherein the distance between two adjacent tower plates is H, the inner diameter of the tower is D, and H is 450 mm; the diameter of the open pore of the outer pipe of the gas distributor is 12mm, the diameter of the open pore of the inner pipe is 8mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.1, the distance between the inlet center of the riser and the centers of the tower plates is 0.2D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.12, the distance between the central line of the downcomer and the centers of the tower plates is 0.4D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.7. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.5, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.4, and the center of the double-ring gas distributor coincides with the center of the tower plate.
Taking the rectification process of the methyl acetate and n-butanol for the preparation of butyl acetate by ester exchange method as an example, as shown in fig. 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 2, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, 38.3kg/h and the reflux ratio of 12, and when the continuous experiment is carried out and the operation is stable, the single-pass conversion rate of the methyl acetate reaches 59.5 percent.
[ example 2 ]
A novel long shaft magnetic pump type reactor is disclosed, as shown in figure 2, the reactor is internally penetrated by 1 long shaft, the long shaft is wrapped by a long sleeve, a bearing is additionally arranged in the reactor, the shaft and the bearing are completely isolated from the outside medium, a paddle soaked in the medium is coupled with the shaft by utilizing the principle of a magnetic pump to realize the stirring effect, each layer of tower plate in the reactor is provided with a riser, the air inlet of the riser is arranged at one side of the long shaft of the reactor, the upper part of the riser is connected with a gas distributor, the center of the gas distributor is arranged on the long shaft, the gas phase from the lower layer of tower plate is uniformly sprayed into a liquid-solid mixture on the tower plate through the gas distributor, each layer of tower plate is provided with a liquid phase inlet and outlet facility, the tower plate is provided with a downcomer, and the liquid phase in the tower flows to the lower layer; the solid particle or particle catalyst is placed on each layer of tower plate, and each layer of tower plate of the reactor is provided with a catalyst loading and unloading opening, so that the catalyst can be replaced without stopping the reactor; wherein the distance between two adjacent tower plates is H, the inner diameter of the tower is D, and H is 300 mm; the diameter of the open pore of the outer pipe of the gas distributor is 2mm, the diameter of the open pore of the inner pipe is 1mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.05, the distance between the inlet center of the riser and the centers of the tower plates is 0.1D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.08, the distance between the central line of the downcomer and the centers of the tower plates is 0.2D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.4. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.3, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.2, and the center of the double-ring gas distributor coincides with the center of the tower plate.
The reaction and rectification process for preparing butyl acetate by transesterification of methyl acetate and n-butanol is taken as an example according to the conditions and steps of example 1, and is shown in figure 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 1, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, 38.3kg/h and 14 reflux ratio, and when the continuous experiment is carried out and the operation is stable, the single-pass conversion rate of the methyl acetate reaches 58.5 percent.
[ example 3 ]
The conditions and procedure described in example 1 were followed, with a spacing of H between two adjacent trays, a column internal diameter D and a H of 400 mm; the diameter of the open pore of the outer pipe of the gas distributor is 10mm, the diameter of the open pore of the inner pipe is 8mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.1, the distance between the inlet center of the riser and the centers of the tower plates is 0.2D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.25, the distance between the central line of the downcomer and the centers of the tower plates is 0.45D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.7. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.5, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.4, and the center of the double-ring gas distributor coincides with the center of the tower plate.
Taking the rectification process of the methyl acetate and n-butanol for the preparation of butyl acetate by ester exchange method as an example, as shown in fig. 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 2, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, 38.3kg/h and the reflux ratio of 12, and when the continuous experiment is carried out and the operation is stable, the single-pass conversion rate of the methyl acetate reaches 58.6 percent.
[ example 4 ]
According to the conditions and procedures described in example 1, the distance between two adjacent trays is H, the internal diameter of the column is D, and H is 500 mm; the diameter of the open pore of the outer pipe of the gas distributor is 15mm, the diameter of the open pore of the inner pipe is 10mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.15, the distance between the inlet center of the riser and the centers of the tower plates is 0.15D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.1, the distance between the central line of the downcomer and the centers of the tower plates is 0.3D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.7. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.5, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.4, and the center of the double-ring gas distributor coincides with the center of the tower plate.
Taking the rectification process of the methyl acetate and n-butanol for the preparation of butyl acetate by ester exchange method as an example, as shown in fig. 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 2, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, kg/h, reflux ratio of 12, continuous experiment, stable operation, methyl acetate conversion per pass of 59.5%.
[ example 5 ]
The conditions and procedure described in example 1 were followed, with a spacing of H between two adjacent trays, a column internal diameter D and a H of 600 mm; the diameter of the open pore of the outer pipe of the gas distributor is 15mm, the diameter of the open pore of the inner pipe is 10mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.2, the distance between the inlet center of the riser and the centers of the tower plates is 0.3D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.1, the distance between the central line of the downcomer and the centers of the tower plates is 0.4D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.9. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.7, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.6, and the center of the double-ring gas distributor coincides with the center of the tower plate.
Taking the rectification process of the methyl acetate and n-butanol for the preparation of butyl acetate by ester exchange method as an example, as shown in fig. 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 2, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, 38.3kg/h and the reflux ratio of 12, and when the continuous experiment is carried out and the operation is stable, the single-pass conversion rate of the methyl acetate reaches 60.0 percent.
[ example 6 ]
The conditions and procedures described in example 1 were followed, with a spacing of H between two adjacent trays, a column internal diameter D and a H of 700 mm; the diameter of the open pore of the outer pipe of the gas distributor is 25mm, the diameter of the open pore of the inner pipe is 20mm, and the open pores are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.25, the distance between the inlet center of the riser and the centers of the tower plates is 0.2D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.1, the distance between the central line of the downcomer and the centers of the tower plates is 0.45D, and the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.9. The gas distributor is a double-ring gas distributor, the ratio of the outer pipe diameter a of the double-ring gas distributor to the inner diameter D of the tower is 0.8, the ratio of the inner pipe diameter b to the inner diameter D of the tower is 0.7, and the center of the double-ring gas distributor coincides with the center of the tower plate.
Taking the rectification process of the methyl acetate and n-butanol for the preparation of butyl acetate by ester exchange method as an example, as shown in fig. 3. The specific implementation process is as follows: the catalytic rectification tower (1) is internally provided with 10 tower plates, the type of which is shown in figure 2, and the inner diameter of the tower is 200 mm. The column plates of each layer are filled with the ester exchange random particle type catalyst. Feeding n-butanol (101) into the 2 nd tray of the catalytic rectification tower (1), and feeding methyl acetate (102) into the 10 th tray of the catalytic rectification tower (1). And (3) carrying out countercurrent contact on methyl acetate and n-butanol, and carrying out reaction and separation. The main components of the tower top steam (103) are methyl acetate and methanol, the methyl acetate and the methanol enter a condenser (2) for condensation, condensate (105) enters a reflux tank (3), liquid phase discharged materials (106) of the reflux tank partially flow back (107) to the catalytic rectifying tower (1) through a reflux pump (5), partial extracted materials (110) enter a subsequent separation section, and the separated methyl acetate can be circulated to the catalytic rectifying tower (1) for further ester exchange reaction. A reboiler is arranged at the tower bottom of the catalytic rectifying tower (1) to provide a heat source, the main components of the tower bottom are n-butyl acetate and n-butyl alcohol, the extracted n-butyl acetate (104) from the tower bottom is sent to a subsequent separation and refining section to obtain an n-butyl acetate product, and the recovered n-butyl alcohol can be circulated to the catalytic rectifying tower (1) to perform further ester exchange reaction.
The novel long-shaft magnetic pump type reactor is used as a catalytic rectification device and used as a methyl acetate and n-butyl alcohol ester exchange catalytic rectification tower (1). The operation temperature at the top of the column was 75 ℃ and the operation pressure at the top of the column was 0.12MPa (A). The molar ratio of n-butanol feed (1) to methyl acetate feed (2) was 2: 1, the mass flow rates are respectively as follows: 75kg/h, 38.3kg/h and the reflux ratio of 12, and when the continuous experiment is carried out and the operation is stable, the single-pass conversion rate of the methyl acetate reaches 58.8 percent.
[ COMPARATIVE EXAMPLE ]
In patent CN101219950A, methyl acetate and n-butanol enter a catalytic rectification tower from the top and the bottom of a catalytic reaction zone respectively, the molar ratio of the methyl acetate to the n-butanol is 1, the reaction temperature is 60 ℃, and the conversion rate of the methyl acetate is 58.4% after the operation is stable with a reflux ratio of 15. The catalyst of the catalytic distillation tower is placed in a reaction liquid phase in the form of a catalyst bag, is difficult to replace, has high requirement on the service life of the catalyst, and can achieve the methyl acetate single-pass conversion rate lower than that of the embodiment of the invention.
Claims (7)
1. A long shaft magnetic pump type reactor is characterized in that 1-2 long shafts penetrate through the reactor, the long shafts are wrapped by long sleeves, bearings are additionally arranged inside the reactor to completely isolate the shafts and the bearings from media outside, blades soaked in the media are coupled with the shafts by utilizing the principle of a magnetic pump to realize the stirring effect, gas risers are arranged on each layer of tower plate in the reactor, gas inlets of the gas risers are arranged on one side of the long shafts of the reactor, and the upper part of the riser is connected with a gas distributor, the center of the gas distributor is positioned on the long shaft, the gas phase from the lower tower plate is uniformly sprayed into the liquid-solid mixture on the tower plate through the gas distributor, each layer of tower plate is provided with a liquid phase inlet and outlet facility, liquid phase feed inlets and liquid phase outlets are respectively arranged on two sides of the tower plate, liquid phase of the tower plate enters the lower tower plate outside the tower, or a downcomer is arranged on the tower plate, and liquid phase in the tower flows to the lower tower plate from the upper tower plate; the solid particle or particle catalyst is placed on each layer of tower plate, and each layer of tower plate of the reactor is provided with a catalyst loading and unloading opening, so that the catalyst can be replaced without stopping the reactor; wherein the distance between two adjacent tower plates is H, the inner diameter of the tower is D, D is 200mm, and H ranges from 300mm to 700 mm; the diameter range of the holes of the outer pipe of the gas distributor is 2-25 mm, the diameter range of the holes of the inner pipe is 1-20 mm, and the holes are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower ranges from 0.05 to 0.25, the distance between the center of an inlet of the riser and the center of the tower plate ranges from 0.1 to 0.3D, the ratio of the diameter D of the downcomer to the inner diameter D of the tower ranges from 0.08 to 0.25, the distance between the central line of the downcomer and the center of the tower plate ranges from 0.20 to 0.45D, the downcomer needs to extend below the liquid level of the tower plate, and the height H of the downcomer and the distance H between two adjacent tower plates ranges from 0.4 to 0.9.
2. The long axis magnetic pump reactor as claimed in claim 1, wherein the liquid phase outlet or downcomer inlet is provided with a screen to prevent catalyst from entering the lower tray.
3. The long axis magnetic pump reactor of claim 1, wherein the gas distributor is a ring gas distributor.
4. The long axis magnetic pump reactor as claimed in claim 3, wherein the gas distributor is a double ring gas distributor having a ratio of the outer tube diameter a to the inner diameter D of the column of 0.3 to 0.8, a ratio of the inner tube diameter b to the inner diameter D of the column of 0.2 to 0.7, and the center of the double ring gas distributor coincides with the center of the tray.
5. The long-axis magnetic pump reactor as claimed in claim 4, wherein the distance between two adjacent tower plates is H, the inner diameter of the tower is D, and the range of H is 400-600 mm; the diameter range of the holes of the outer pipe of the gas distributor is 5-20 mm, the diameter range of the holes of the inner pipe is 5-15 mm, and the holes are uniformly distributed at equal intervals; the ratio of the diameter c of the riser to the inner diameter D of the tower is 0.1-0.15; the distance between the center of the riser inlet and the center of the tower plate is 0.1-0.2D; the ratio of the diameter D of the downcomer to the inner diameter D of the tower is 0.1-0.15; the distance between the central line of the downcomer and the center of the tower plate is 0.3-0.4D; the ratio of the height H of the downcomer to the distance H between two adjacent tower plates is 0.6-0.8.
6. The long axis magnetic pump reactor as claimed in claim 1, wherein the reactor is provided with a magnetic pump stirrer.
7. The long axis magnetic pump reactor as claimed in claim 1, wherein the medium is three phases of gas, liquid and solid.
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| CN1079727A (en) * | 1992-01-24 | 1993-12-22 | 旭化成工业株式会社 | The method of mononuclear aromatics partial hydrogenation |
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