CN115124422B

CN115124422B - Equipment for improving ethyl acetate yield

Info

Publication number: CN115124422B
Application number: CN202210740493.7A
Authority: CN
Inventors: 季青松; 冯佩洪; 佟刚; 赵楚榜
Original assignee: Zhuhai Qianxin New Material Co ltd
Current assignee: Zhuhai Qianxin New Material Co ltd
Priority date: 2022-06-28
Filing date: 2022-06-28
Publication date: 2023-06-30
Anticipated expiration: 2042-06-28
Also published as: CN115124422A

Abstract

The invention discloses equipment for improving the yield of ethyl acetate, which comprises a stirring-free combined ethyl acetate esterification reaction kettle, wherein the esterification reaction kettle consists of an esterification kettle and an esterification tower, a baffling mechanism for improving the reaction conversion rate is arranged in the esterification kettle, the baffling mechanism is vertically and equidistantly arranged in the esterification kettle and consists of a horizontal baffling mechanism and a vertical baffling mechanism, a material circulation inlet is arranged at the joint of the esterification kettle and the esterification tower, a feed inlet is arranged on the side surface of the esterification kettle, a circulating material outlet is arranged at the center of the bottom end of the esterification kettle, and the horizontal baffling mechanism comprises a third horizontal baffling plate and a middle baffling plate; the invention has the advantages that the horizontal baffling mechanism and the vertical baffling mechanism are arranged, so that the material reaction time is more uniform, the esterification reaction conversion rate is high, the content of unreacted raw materials is reduced, and the single-tower yield is increased.

Description

Equipment for improving ethyl acetate yield

Technical Field

The invention relates to the technical field of chemical production equipment, in particular to equipment for improving the yield of ethyl acetate.

Background

In the chemical production process, the domestic common flow of pressurized ethyl ester line esterification is as follows: raw materials of acetic acid and ethanol enter the bottom of the esterification tower in proportion, react under the action of a catalyst, the tower bottom material is conveyed to a reboiler through a circulating pump to be heated and then returned to the bottom of the esterification tower, a certain reaction temperature is maintained for reaction, an azeotrope is formed in the esterification tower, and the mixture is distilled out from the top of the esterification tower.

The following problems exist in practical use:

(1) Raw materials are immediately dispersed after entering the lower part of the reaction tower, the concentration is reduced, the reaction time of the materials in the reaction kettle is greatly different due to lack of stirring, and the uneven reaction causes poor crude ester content (high alcohol content and high side reaction impurities);

(2) The gasification rate of the reboiler is low, most of the reaction materials form flash evaporation in the esterification tower and then return to the esterification tower bottom again to react with the feed again, and the problems of large reaction time difference and unstable crude ester content caused by uneven mixing are also existed.

The above defects may result in a decrease in the esterification rate of ethyl acetate, thereby affecting the yield of ethyl acetate per unit time.

Therefore, it is desirable to find a device to solve the above-mentioned problems.

Disclosure of Invention

The invention aims to provide equipment for improving the yield of ethyl acetate so as to solve the defects.

In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides a promote equipment of ethyl acetate productivity, includes not having the ethyl acetate esterification reaction cauldron of stirring combination formula, esterification reaction cauldron comprises esterification kettle and esterification tower, the inside baffling mechanism that is used for improving reaction conversion rate that is provided with of esterification kettle, baffling mechanism is in the inside perpendicular equidistance setting of esterification kettle, baffling mechanism includes horizontal baffling mechanism and perpendicular baffling mechanism.

Further, a material circulation inlet is formed in the joint of the esterification kettle and the esterification tower, a feed inlet is formed in the side face of the esterification kettle, and a circulating material outlet is formed in the center of the bottom end.

Further, the horizontal baffle mechanism comprises a third horizontal baffle plate and a middle baffle plate, wherein the middle baffle plate is overlapped with the third horizontal baffle plate, a side baffle plate is arranged between overlapped ends, and the third horizontal baffle plate is uniformly provided with downflow holes in an overlapped area of the third horizontal baffle plate and the middle baffle plate.

Further, the vertical baffle mechanism comprises a receiving plate which is overlapped with the middle baffle plate, a third downflow interval is arranged at one end of the receiving plate extending out of the middle baffle plate, third vertical baffle plates are horizontally and equidistantly arranged in the third downflow interval, the third vertical baffle plates are vertically in a corrugated structure, side baffles are arranged at the overlapping ends of the middle baffle plates and the receiving plate, and downflow holes are uniformly formed in the overlapping areas.

Furthermore, the middle baffle plate is at least provided with two groups, the mutually overlapped ends are provided with side baffles, and the mutually overlapped area parts are uniformly provided with downflow holes.

Further, the horizontal baffle mechanism comprises a first horizontal baffle plate, the vertical baffle mechanism comprises a first downflow section arranged at the end part of the first horizontal baffle plate, first vertical baffle plates are horizontally and equidistantly arranged in the first downflow section, and the first vertical baffle plates are vertically in a corrugated structure.

Further, the horizontal baffle mechanism comprises a second horizontal baffle plate, and the surface of the second horizontal baffle plate is uniformly provided with corrugated grooves to form a corrugated structure.

Further, the vertical baffle mechanism comprises a second downflow section arranged at the end part of the corrugated groove, second vertical baffles are horizontally and equidistantly arranged in the second downflow section, and the second vertical baffles are vertically in a corrugated structure.

Further, the horizontal baffle mechanisms and the vertical baffle mechanisms in the two vertically adjacent baffle mechanisms are staggered in a shape like a Chinese character' each.

Further, the horizontal baffling mechanism and the vertical baffling mechanism are combined into an integrated structure, and are installed inside the esterification kettle in a circular shape, and the overlooking width ratio of the horizontal baffling mechanism to the vertical baffling mechanism is 3-8:1.

Compared with the prior art, the invention has the beneficial effects that:

the invention can slow down the downward flowing trend of materials in the horizontal direction by arranging the horizontal baffling mechanism and the vertical baffling mechanism, so that the materials can be fully contacted on the surface of the horizontal baffling mechanism to ensure uniform reaction time, and simultaneously, the corrugated vertical baffling mechanism is utilized to ensure that the materials are mixed and contacted again in the downward flowing process to ensure that the reaction is close to the tubular reaction, thereby ensuring that the reaction time of the materials is more uniform, the esterification reaction conversion rate is high, the unreacted raw material content is reduced, and the yield of a single tower is increased.

Drawings

FIG. 1 is a schematic structural diagram of a reaction kettle according to an embodiment of the present invention;

FIG. 2 is a schematic cross-sectional view of section A-A of the embodiment of FIG. 1;

FIG. 3 is a schematic diagram of the internal structure of the esterification reactor in the embodiment of FIG. 1;

FIG. 4 is a schematic view of the baffle mechanism of embodiment 2 of FIG. 1;

FIG. 5 is a schematic side view of the baffle mechanism of embodiment 2 of FIG. 1;

FIG. 6 is a schematic view of the baffle mechanism of embodiment 3 of FIG. 1;

FIG. 7 is a schematic side view of the baffle mechanism of embodiment 3 of FIG. 1;

FIG. 8 is a schematic view of the baffle mechanism of embodiment 1 of FIG. 1;

FIG. 9 is a schematic top view of the baffle mechanism of embodiment 1 of FIG. 1;

FIG. 10 is a schematic view of the baffle mechanism of embodiment 1 of FIG. 1 in a bottom view;

FIG. 11 is a schematic diagram showing the structure of the esterification reaction scheme in the embodiment of FIG. 1.

Description of the drawings: 1. an esterification kettle; 2. an esterification tower; 3. a first horizontal baffle; 4. a first downstream interval; 5. a first vertical baffle; 6. a material circulation inlet; 7. a feed inlet; 8. a circulating material outlet; 9. a second horizontal baffle; 10. a corrugated groove; 11. a second downstream interval; 12. a second vertical baffle; 13. a third horizontal baffle; 14. a downflow hole; 15. side baffles; 16. an intermediate baffle; 17. a receiving plate; 18. a third downstream interval; 19. a third vertical baffle; 20. a reboiler; 21. and a circulation pump.

Detailed Description

The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Example 1:

referring to fig. 1-11, an apparatus for increasing ethyl acetate yield includes a combined ethyl acetate esterification reaction kettle without stirring, wherein the esterification reaction kettle is composed of an esterification kettle 1 (with a size of 4m in diameter and a height of 11.2 m) and an esterification tower 2 (with a size of 3m in diameter and a height of 33.7 m), a baffle mechanism for increasing reaction conversion rate is arranged inside the esterification kettle 1, and the baffle mechanism is vertically and equidistantly arranged inside the esterification kettle 1 and comprises a horizontal baffle mechanism and a vertical baffle mechanism;

wherein, a material circulation inlet 6 is arranged at the joint of the esterification kettle 1 and the esterification tower 2, a feed inlet 7 is arranged on the side surface of the esterification kettle 1, and a circulation material outlet 8 is arranged at the center of the bottom end;

wherein the horizontal baffling mechanisms and the vertical baffling mechanisms in the two vertically adjacent baffling mechanisms are staggered in a shape like a Chinese character 'each other';

in the esterification reaction process, raw material acetic acid, ethanol and catalytic amount of concentrated sulfuric acid are added through a feed port 7, so that the raw material acetic acid, ethanol and catalytic amount of concentrated sulfuric acid enter the esterification kettle 1 in proportion, meanwhile, under the action of a horizontal baffling mechanism and a vertical baffling mechanism, materials flowing through the bottom of the esterification kettle 1 are gradually and uniformly mixed in the process of automatically flowing, materials flowing through a circulating material outlet 8 are conveyed to a reboiler 20 through a circulating pump 21, and the reboiler 20 is heated by external steam, so that the materials react in the reboiler 20, and then return to the esterification kettle 1 through a material circulating inlet 6, and the materials in the esterification kettle 1 and the reboiler 20 are circulated in such a way that the materials react gradually and completely, and then are distilled and purified through an esterification tower 2.

The horizontal baffling mechanism and the vertical baffling mechanism are combined into an integrated structure, the combination is installed in the esterification kettle 1 in a circular shape, meanwhile, the overlooking width ratio of the horizontal baffling mechanism to the vertical baffling mechanism is 3-8:1, the 3:1 ratio is selected in the embodiment, sufficient baffling time can be ensured, and meanwhile, the flow of materials can not be blocked.

In order to improve the baffling effect, the horizontal baffling mechanism comprises a third horizontal baffling plate 13 and a middle baffling plate 16, wherein the middle baffling plate 16 is overlapped with the third horizontal baffling plate 13, a side baffle 15 is arranged between overlapped ends, and the third horizontal baffling plate 13 is uniformly provided with a down-flow hole 14 in the overlapped area of the third horizontal baffling plate 13 and the middle baffling plate 16;

meanwhile, the vertical baffle mechanism comprises a bearing plate 17 overlapped with the middle baffle plate 16, a third downflow interval 18 is arranged at one end of the bearing plate 17 extending out of the middle baffle plate 16, third vertical baffle plates 19 are horizontally and equidistantly arranged in the third downflow interval 18, the third vertical baffle plates 19 are vertically in a corrugated structure, side baffles 15 are also arranged at the overlapped ends of the middle baffle plate 16 and the bearing plate 17, and downflow holes 14 are uniformly formed in the overlapped area.

Wherein, the middle baffle plate 16 is provided with at least two groups, in the embodiment, two groups are provided, the mutually overlapped ends are provided with side baffle plates 15, and the mutually overlapped area parts are uniformly provided with the downflow holes 14;

in the practical use process, the combination of the third horizontal baffle plate 13, the middle baffle plate 16 and the bearing plate 17 is in a ladder-shaped structure, meanwhile, one end far away from the bearing plate 17 is provided with a side baffle plate 15 to block raw material fluid, and the top of the overlapped part is provided with a down-flow hole 14, so that when the raw material fluid falls on the surface of the third horizontal baffle plate 13, a part of the raw material fluid falls on the surface of the middle baffle plate 16 along the third horizontal baffle plate 13, a part of the raw material fluid flows on the surface of the middle baffle plate 16 along the down-flow hole 14, and flows on the surface of the middle baffle plate 16 again through the circulation, and finally flows into the area of the third down-flow interval 18, the raw material can be fully mixed in the down-flow process, the contact time between the reaction material and the catalyst is greatly improved, and the reaction time is improved, so that the reaction of the raw material is more fully and uniformly;

secondly, when entering into the region of the third downflow interval 18, the third vertical baffle plates 19 which are arranged at equal intervals can vertically and uniformly disperse and downflow the material fluid, and the corrugated structure of the third vertical baffle plates is utilized to mix the material fluid again and mix the unreacted and complete material again, so that the reaction efficiency is improved, and meanwhile, the downflow of the material fluid is more uniform.

Example 2:

referring to fig. 1-11, the present embodiment is basically the same as the embodiment 1, except that:

in order to improve the baffling effect, the horizontal baffling mechanism comprises a first horizontal baffling plate 3, the vertical baffling mechanism comprises a first downflow interval 4 arranged at the end part of the first horizontal baffling plate 3, first vertical baffling plates 5 are horizontally and equidistantly arranged in the first downflow interval 4, and the first vertical baffling plates 5 are vertically in a corrugated structure;

in the actual use process, the first horizontal baffle plate 3 can carry out the bearing and retarding of the material fluid, so that the material fluid is fully contacted with the surface of the first horizontal baffle plate 3, the reaction time is improved, the material reaction is more fully and uniformly carried out, meanwhile, when the material fluid enters the first downflow interval 4 area, the material fluid is vertically and uniformly dispersed and downflow through the first vertical baffle plates 5 which are equidistantly arranged, the material fluid is mixed again by utilizing the corrugated structure of the material fluid, and the unreacted complete material is mixed again, so that the reaction efficiency is improved, and meanwhile, the downflow of the material fluid is more uniform;

compared with the embodiment 1, the embodiment has lower material mixing degree, but the fluid downflow velocity is improved, and the method can be suitable for different production environments and requirements.

Example 3:

in order to improve the baffling effect, the horizontal baffling mechanism comprises a second horizontal baffling plate 9, and the surface of the second horizontal baffling plate 9 is uniformly provided with corrugated grooves 10 to form a corrugated structure.

Meanwhile, the vertical baffle mechanism comprises a second downflow interval 11 arranged at the end part of the corrugated groove 10, second vertical baffle plates 12 are horizontally and equidistantly arranged in the second downflow interval 11, and the second vertical baffle plates 12 are vertically in a corrugated structure;

in the actual use process, the second horizontal baffle plate 9 can carry out carrying retarding on the material fluid, meanwhile, the second horizontal baffle plate 9 is in a corrugated structure due to the arrangement of the corrugated grooves 10, so that the material fluid is fully contacted with the surface of the second horizontal baffle plate 9, the reaction time is improved, the material reaction is more fully and uniformly carried out, meanwhile, when the material fluid enters the second downflow zone 11, the material fluid can be vertically and uniformly dispersed and downflow through the second vertical baffle plates 12 which are equidistantly arranged, and the material fluid is mixed again due to the corrugated structure, and the materials which are completely reacted are mixed again, so that the reaction efficiency is improved, and meanwhile, the downflow of the material fluid is more uniform;

compared with example 1, the material mixing degree of the embodiment is lower, but the fluid downflow velocity is improved, compared with example 2, the material mixing degree of the embodiment is higher, but the fluid downflow velocity is reduced, and the method can be suitable for different production environments and requirements.

Comparative example 1

Comparative example 1 adopts a similar structure to example 1, which differs from the apparatus in example 1 in that the esterification vessel 1 in comparative example 1 does not contain any baffle mechanism structure.

Test case

To test the ethyl acetate yields of the apparatus of example 1 and comparative example 1, the following tests were made, respectively:

raw material acetic acid and ethanol are taken, the feeding amounts of the raw material acetic acid and the ethanol are adjusted, the raw material acetic acid and the ethanol are respectively fed from a feed inlet 7 of the example 1 and a feed inlet 7 of the comparative example 1, the feeding rates are 18500kg/h and 15250kg/h respectively, an equal amount of concentrated sulfuric acid is added, and steam is externally supplied to heat a reboiler 20 to 105 ℃ to enable the raw materials to start reacting, and the zero point of the reaction is set at the moment.

Sampling and testing the esterification rate of the materials in the reaction kettle respectively at 5min, 10min, 15min, 20min and the like after zero crossing, as shown in table 1.

TABLE 1 specific time node, material esterification rates (%)

	5min	10min	15min	20min
					Example 1	34.9％	44.1％	51.4％	54.9％
Comparative example 1	31.2％	39.8％	45.1％	49.4％

From the data in Table 1, it can be seen that the examples have higher esterification rates and faster reaction rates than the comparative examples. And the higher esterification rate in unit time means that the raw material reaction is more sufficient, and the steam unit consumption is less.

It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides a promote equipment of ethyl acetate productivity, includes no stirring combination formula ethyl acetate esterification reaction cauldron, its characterized in that: the esterification reaction kettle consists of an esterification kettle (1) and an esterification tower (2), wherein a baffling mechanism for improving the reaction conversion rate is arranged in the esterification kettle (1), the baffling mechanism is vertically and equidistantly arranged in the esterification kettle (1), and the baffling mechanism comprises a horizontal baffling mechanism and a vertical baffling mechanism;

the horizontal baffle mechanism comprises a third horizontal baffle plate (13) and a middle baffle plate (16), wherein the middle baffle plate (16) is overlapped with the third horizontal baffle plate (13), a side baffle plate (15) is arranged between overlapped ends, and lower circulation holes (14) are uniformly formed in the overlapped area of the third horizontal baffle plate (13) and the middle baffle plate (16) by the third horizontal baffle plate (13);

the vertical baffle mechanism comprises a bearing plate (17) overlapped with the middle baffle plate (16), a third downflow interval (18) is arranged at one end, extending out of the middle baffle plate (16), of the bearing plate (17), third vertical baffle plates (19) are horizontally and equidistantly arranged in the third downflow interval (18), the third vertical baffle plates (19) are vertically in a corrugated structure, side baffles (15) are also arranged at the overlapped ends of the middle baffle plate (16) and the bearing plate (17), and downflow holes (14) are uniformly formed in the overlapped areas;

a material circulation inlet (6) is arranged at the joint of the esterification kettle (1) and the esterification tower (2), a feed inlet (7) is arranged on the side surface of the esterification kettle (1), and a circulation material outlet (8) is arranged at the center of the bottom end;

wherein the horizontal baffling mechanisms and the vertical baffling mechanisms in the two vertically adjacent baffling mechanisms are staggered in a shape of a Chinese character 'each other';

the horizontal baffling mechanism and the vertical baffling mechanism are combined into an integrated structure, the integrated structure is installed inside the esterification kettle (1) in a circular shape, and the overlooking width ratio of the horizontal baffling mechanism to the vertical baffling mechanism is 3-8:1.

2. An apparatus for increasing the yield of ethyl acetate according to claim 1, characterized in that said intermediate baffles (16) are provided in at least two groups and are provided with side baffles (15) at mutually coinciding ends, and in that the mutually coinciding areas are provided with evenly distributed lower flow openings (14).

3. An apparatus for increasing ethyl acetate yield according to claim 1, characterized in that the horizontal baffle means comprises a first horizontal baffle plate (3), the vertical baffle means comprises a first downflow section (4) arranged at the end of the first horizontal baffle plate (3), the first vertical baffle plate (5) is horizontally and equidistantly arranged inside the first downflow section (4), and the first vertical baffle plate (5) is vertically corrugated.

4. The equipment for improving the yield of ethyl acetate according to claim 1, wherein the horizontal baffle mechanism comprises a second horizontal baffle plate (9), and corrugated grooves (10) are uniformly formed on the surface of the second horizontal baffle plate (9) to form a corrugated structure.

5. An apparatus for increasing the yield of ethyl acetate according to claim 4 wherein said vertical baffle means comprises a second downflow section (11) provided at the end of said corrugation (10), said second downflow section (11) being internally and horizontally equally spaced with a second vertical baffle (12), said second vertical baffle (12) being vertically corrugated.