APPARATUS AND METHOD FOR ESTERIFICATION REACTION
20220314186 · 2022-10-06
Inventors
- Yeon Uk Choo (Daejeon, KR)
- Sung Kyu Lee (Daejeon, KR)
- Hyoung Jun (Daejeon, KR)
- Hyun Kyu Kim (Daejeon, KR)
- Chan Hyu Jin (Daejeon, KR)
- Jin Sung Park (Daejeon, KR)
Cpc classification
B01J2219/00182
PERFORMING OPERATIONS; TRANSPORTING
B01J19/18
PERFORMING OPERATIONS; TRANSPORTING
B01J19/24
PERFORMING OPERATIONS; TRANSPORTING
C07C67/08
CHEMISTRY; METALLURGY
B01J2219/00159
PERFORMING OPERATIONS; TRANSPORTING
B01J19/0013
PERFORMING OPERATIONS; TRANSPORTING
C07C67/08
CHEMISTRY; METALLURGY
International classification
B01J19/00
PERFORMING OPERATIONS; TRANSPORTING
B01J19/24
PERFORMING OPERATIONS; TRANSPORTING
Abstract
An esterification reaction apparatus and an esterification reaction method, the esterification reaction apparatus comprising a reaction tank having an accommodation part, in which a raw material containing carboxylic acid and alcohol is accommodated, a heating unit configured to individually heat partition regions that are partitioned into N regions in a vertical direction of the accommodation part, and a controller configured to control the heating unit so that only the partition regions in which a liquid is accommodated among the N partition regions are heated, thereby performing an esterification reaction of the raw material.
Claims
1. An esterification reaction apparatus, comprising: a reaction tank having an accommodation part in which a raw material containing carboxylic acid and alcohol is accommodated; a heating unit configured to individually heat partition regions that are partitioned into N regions in a vertical direction of the accommodation part, where N is an integer of 2 or more; and a controller configured to control the heating unit so that only the partition regions in which a liquid of the raw material is accommodated among the N partition regions are heated, thereby performing an esterification reaction of the raw material.
2. The esterification reaction apparatus of claim 1, wherein the heating unit comprises N heat source supply parts, which are respectively provided in the N partition regions.
3. The esterification reaction apparatus of claim 2, wherein each of the heat source supply parts comprises a heat source supply tube therein which has the form of a coil and through which a high-temperature fluid passes, wherein the high-temperature fluid is a heat source.
4. The esterification reaction apparatus of claim 3, wherein the heat source supply parts comprise a plurality of heat source supply tubes wound in the form of the coil, which have different winding widths from the center axis in the vertical direction of the accommodation part from each other.
5. The esterification reaction apparatus of claim 4, wherein the plurality of heat source supply tubes are provided in a shape of being wound multiple times around the vertical central axis of the accommodation part in the reaction tank.
6. The esterification reaction apparatus of claim 3, wherein a coil pitch of each of the heat source supply tubes disposed in the partition region, which is disposed at the lowermost portion among the N partition regions, is equal to or less than a coil pitch of each of the heat source supply tubes disposed in the remaining regions.
7. The esterification reaction apparatus of claim 3, wherein the high-temperature fluid comprises steam.
8. The esterification reaction apparatus of claim 3, further comprising a sensing unit configured to sense a liquid-accommodated state in the N partition regions, wherein the sensing unit is configured to transmit information of the sensed liquid-accommodated state to the controller.
9. The esterification reaction apparatus of claim 8, wherein the sensing unit comprises a liquid level sensor disposed in the reaction tank to measure an accommodation height (level) of the liquid accommodated in the accommodation part.
10. The esterification reaction apparatus of claim 9, wherein the controller is configured to determine whether the liquid is accommodated in each of the N partition regions of the accommodation part through sensed accommodation level values of the accommodated liquid sensed through the sensing unit so that the high-temperature liquid is supplied to the heat source supply tubes of the partition regions which are determined to contain the liquid among the N partition regions, and supplying the high-temperature liquid to the heat source supply tubes of the partition regions which are determined to contain no liquid among the N partition regions is blocked.
11. An esterification reaction method comprising: a supply process of supplying a raw material containing carboxylic acid and alcohol to an accommodation part of a reaction tank; a heating process of individually heating partition regions that are partitioned into N regions in a vertical direction of the accommodation part through a heating unit, where N is an integer of 2 or more; and a control process of controlling the heating unit through a controller during the heating process so that only the partition regions in which a liquid of the raw material is accommodated among the N partition regions are heated, thereby performing an esterification reaction of the raw material.
12. The esterification reaction method of claim 11, wherein, in the heating process, the partition regions of the accommodation part are individually heated through the N heat source supply parts constituting the heating unit, which are respectively provided in the N partition regions.
13. The esterification reaction method of claim 12, wherein, in the heating process, the partition regions of the accommodation part are individually heated using heat source supply tubes, each of which has the form of a coil and through which a high-temperature fluid passes therein, as the heat source supply parts, wherein the high-temperature fluid is a heat source.
14. The esterification reaction method of claim 13, wherein, in the heating process, steam is used as the high-temperature fluid passing through the heat source supply tubes.
15. The esterification reaction method of claim 13, further comprising a sensing process of individually sensing liquid-accommodated states in the N partition regions through a sensing unit, wherein, in the sensing process, information of the liquid-accommodated states, which are sensed through the sensing unit, are transmitted to the controller.
16. The esterification reaction method of claim 15, wherein, in the sensing process, an accommodated level (height) of the liquid accommodated in the accommodation part is sensed through a liquid level sensor, which is the sensing unit and disposed in the reaction tank.
17. The esterification reaction method of claim 16, wherein, in the control process, the controller determines whether the liquid is accommodated in each of the partition regions of the accommodation part through sensed accommodation level values of the accommodated liquid, which are sensed through the sensing unit so that the high-temperature liquid is supplied to the heat source supply tubes of the partition regions, which are determined to contain the liquid among the N partition regions, and supplying the high-temperature liquid to the heat source supply tubes of the partition regions, which are determined to contain no liquid among the N partition regions, is blocked.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0013]
[0014]
[0015]
[0016]
[0017]
DETAILED DESCRIPTION
[0018] The objectives, specific advantages, and novel features of the present invention will become more apparent from the following detailed description taken in conjunction with the accompanying drawings. It should be noted that the reference numerals are added to the components of the drawings in the present specification with the same numerals as possible, even if they are illustrated in other drawings. Also, the present invention may be embodied in different forms and should not be construed as limited to the embodiments set forth herein. In the following description of the present invention, the detailed descriptions of related arts which may unnecessarily obscure the gist of the present invention will be omitted.
[0019]
[0020]
[0021] Referring to
[0022] In more detail, the reaction tank 110 comprises an accommodation part 111 in which the raw material containing carboxylic acid and alcohol, which are supplied from the outside, is accommodated.
[0023] Here, the carboxylic acid may comprise, for example, one or more materials selected from the group consisting of terephthalic acid, phthalic acid, isophthalic acid, and cyclohexane dicarboxylic acid.
[0024] Here, the alcohol may have 3 to 10 alkyl carbon atoms.
[0025] The raw material may be supplied from the outside of the reaction tank 110 to the accommodation part 111 of the reaction tank 110 through a raw material supply part 150. Here, the raw material supplied to the accommodation part 111 of the reaction tank 110 may be stirred through a stirrer 180 disposed in the accommodation part 111 of the reaction tank 110. Here, a first control valve 151 is provided in the raw material supply part 150 to control the supply of the raw material.
[0026] The heating unit 120 may individually heat each of the partition regions N, N−1, and N−2, which are divided into N (N is an integer of 2 or more) regions in a vertical direction of the accommodation part 111. (Although three partition regions are shown in
[0027] Also, the heating unit 120 may comprise N heat source supply parts 121, 122, and 123, which are respectively provided in the N partition regions N, N−1, and N−2. Here, the heating unit 120 may further comprise a supply part valve V for opening and closing each of the N heat source supply parts 121, 122, and 123.
[0028] Furthermore, the heating unit 120 may comprise, for example, a first heat source supply part 121 disposed in an upper portion of the accommodation part 111 in the vertical direction, a second heat source supply part 122 disposed at a central portion of the accommodation part 111, and a third heat source supply part 123 disposed in a lower portion of the accommodation part 111, but the number of heat source supply parts 121, 122, and 123 of the heating unit 120 is not necessarily limited thereto. Here, the heating unit 120 may comprise, for example, a first supply part valve V1 for opening and closing the first heat source supply part 121, a second supply part valve V2 for opening and closing the second heat source supply part 122, and a third supply part valve V3 for opening and closing the third heat source supply part 123.
[0029] Referring to
[0030] Also, the heat source supply part 121, 122, and 123 may comprise a plurality of heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c wound in the form of the coil around a vertical central axis X, which have different winding widths a, b, and c. Here, each of the N heat source supply parts 121, 122, and 123 may comprise the plurality of heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, each of which has the form of the coil. Thus, it is possible to uniformly heat the accommodation part 111 of the reaction tank 110. Here, the heat source supply parts 121, 122, and 123 disposed in the partition regions N, N−1, and N−2 of the accommodation part 111, which supplies the heat source, among the N heat source supply parts 121, 122, 123, may uniformly heat the corresponding partition regions N, N−1, and N−2.
[0031] Furthermore, the plurality of heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may comprise, for example, first heat source supply tubes 121a, 122a, and 123a and second heat source supply tubes 121b, 122b, and 123b, and third heat source supply tubes 121c, 122c, and 123c, which are arranged in an order of having the largest winding widths a, b, and c. That is, the first heat source supply tubes 121a, 122a, and 123a, each of which has the largest winding width a, are disposed in a spiral curve shape to be closest to the reaction tank 110, the third heat source supply tubes 121c, 122c, and 123c, each of which has the smallest winding width c, are disposed in a helical curve shape to be closest to the vertical central axis X of the accommodation part 111, and the second heat source supply tubes 121b, 122b, 123b, each of which has the winding width b, between the first heat source supply tubes 121a, 122a, 123a and the third heat source supply tubes 121c, 122c, and 123c are disposed in a spiral curve shape between the first heat source supply tubes 121a, 122a, 123a and the third heat source supply tubes 121c, 122c, and 123c. However, the number of heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the heat source supply parts 121, 122, and 123 is not necessarily limited thereto.
[0032] Also, the plurality of heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may be provided, for example, in a shape of being wound multiple times around the vertical central axis X of the accommodation part 111 in the reaction tank 110.
[0033] Also, a coil pitch P of each of the heat source supply tubes 123a, 123b, and 123c disposed in the partition region N−2, which is disposed at the lowermost portion, among the N partition regions N, N−1, and N−2 of the accommodation part 111 may be equal to or less than a coil pitch P of each of the heat source supply tubes 121a, 122a, 121b, 122b, 121c, and 122c, which are disposed in the remaining regions N and N−1. Therefore, heat transfer efficiency in the lowermost partition region N−2 of the accommodation part 111, in which the liquid raw material is accommodated always, may be more improved to improve the reaction efficiency.
[0034] The carboxylic acid and the alcohol, which are heated through the heating unit 120, may cause an esterification reaction to generate an ester-based material and water as products of the esterification reaction. Here, the liquid ester-based material may be generated by the esterification reaction and then be discharged to the outside of the reaction tank 110 through a liquid material discharge part 160, and the water may be generated, but be vaporized to be discharged to the outside of the reaction tank 110 through a vaporized material discharge part 170.
[0035] For example, the liquid material discharge part 160 may be connected to a lower portion of the reaction tank 110, and the vaporized material discharge part 170 may be connected to an upper portion of the reaction tank 110.
[0036] Also, a second control valve 161 may be provided in the liquid material discharge part 160 to control the discharge of the generated liquid material, and a third control valve 171 may be provided in the vaporized material discharge part 170 to control the discharge of the vaporized material. (see
[0037] Referring to
[0038] In addition, the sensing unit 140 may transmit the sensed liquid-accommodated state information to the controller 130.
[0039] Furthermore, the sensing unit 140 may comprise liquid level sensors 141 and 142 that are disposed inside the reaction tank 110 to measure an accommodation height (level) of a liquid R accommodated in the accommodation part 111.
[0040] Here, the sensing unit 140 may comprise a first liquid level sensor 141 disposed in the upper portion of the accommodation part 111 of the reaction tank 110 and a second liquid level sensor 142 disposed in the lower portion of the accommodation part 111 of the reaction tank 110.
[0041] Referring to
[0042] In addition, the controller 130 may determine whether the liquid is accommodated in each of the partition regions N, N−1, and N−2 of the accommodation part 111 through sensed accommodation level values of the accommodated liquid R, which are sensed through the sensing unit 140. Here, the controller 130 may control the supply of the high-temperature liquid so that the high-temperature liquid is supplied to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain the liquid R, among the N partition regions N, N−1, N−2, and the supply of the high-temperature liquid to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain no liquid R, among the N partition regions N, N−1, N−2 is blocked.
[0043] Here, the partition regions N, N−1, and N−2, which are heated by supplying the high-temperature fluid to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, may be heated, for example, at a temperature of 150° C. to 230° C. Here, particularly, the partition regions N, N−1, and N−2, which are heated by supplying the high-temperature fluid to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, may be heated, for example, at a temperature of 180° C. Here, the opening and closing of each of the supply part valves V1, V2, and V3 may be controlled by the controller 130 so that the corresponding partition regions N, N−1, and N−2 are individually heated through the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, which constituent the heating unit 120.
[0044] The controller 130 may be connected to the raw material supply part 150 through the first control valve 151, connected to the liquid martial discharge part 160 through the second control valve 161, and connected to the vaporized material discharge part 170 through the third control valve 171 to control the first control valve 151, the second control valve 161, and the third control valve 171. (Here, since the technology in which the valve is electrically controlled through the controller is a known technology, descriptions of the operation principle and control principle of the valve will be omitted)
[0045] Referring to
[0046] Accordingly, the heat source may be supplied to only the wet region, in which the liquid R is accommodated, among the N partition regions N, N−1, and N−2 of the accommodation part 111 to significantly improve the heat transfer efficiency. That is, when the heat is applied to the raw material mixed with liquid carboxylic acid and alcohol to cause the esterification reaction, only the region in which the raw material solution, in which the carboxylic acid and the alcohol are mixed, is accommodated to cause the esterification reaction may be heated to prevent a problem in which the heat source is unnecessarily applied to the region in which the raw material solution is not accommodated so as not to cause the esterification reaction, to deteriorate the efficiency.
[0047] Also, the supply of the heat source to a dry region in which the liquid R is not accommodated may be blocked to prevent the raw material from being carbonized. That is, when the heat is applied to the raw material mixed with the liquid carboxylic acid and the alcohol to cause the esterification reaction, a problem, in which the heat is applied to a solid or gaseous material in the raw material to carbonize the solid or gaseous material, thereby generating foreign substances, may be prevented by blocking the supply of the heat source to the dry region.
[0048] Hereinafter, an esterification reaction method according to an embodiment of the present invention will be described.
[0049] Referring to
[0050] In more detail, in the supply process, the raw material containing carboxylic acid and alcohol may be supplied to the accommodation part 111 of the reaction tank 110.
[0051] In addition, in the supply process, for example, the liquid carboxylic acid and alcohol may be mixed and supplied to the accommodation part 111 of the reaction tank 110 through a raw material supply part 150. Here, a first control valve 151 is provided in the raw material supply part 150 to control the supply of the raw material.
[0052] The carboxylic acid may comprise, for example, one or more materials selected from the group consisting of terephthalic acid, phthalic acid, isophthalic acid, and cyclohexane dicarboxylic acid.
[0053] The alcohol may have 3 to 10 alkyl carbon atoms.
[0054] Also, a molar ratio of an amount of added carboxylic acid and a total amount of added alcohol to the accommodation part 111 of the reaction tank 110 during the supply process may be, for example, 1:2 to 1:5.
[0055] In the heating process, the partition regions N, N−1, and N−2 that are divided into N (N is an integer of 2 or more) regions in a vertical direction of the accommodation part 111 may be individually heated through the heating unit 120.
[0056] In addition, in the heating process, the partition regions N, N−1, and N−2 of the accommodation part 111 may be individually heated through N heat source supply parts 121, 122, and 123 constituting the heating unit 120, which are respectively provided in N partition regions N, N−1, and N−2.
[0057] Furthermore, the partition regions N, N−1, and N−2 of the accommodation part 111 may be individually heated using heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, each of which has the form of a coil and through which a high-temperature fluid, that is the heat source, passes, in the heat source supply parts 121, 122, and 123.
[0058] In addition, in the heating process, steam may be used as the high-temperature fluid passing through the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c.
[0059] The carboxylic acid and the alcohol may cause the esterification reaction through the heating process to generate an ester-based material and water as products of the esterification reaction.
[0060] Here, the liquid ester-based material, which is generated through the esterification reaction, may be discharged to the outside of the reaction tank 110 through a liquid material discharge part 160, and the water may be vaporized to be discharged to the outside of the reaction tank 110 through a vaporized material discharge part 170.
[0061] For example, the liquid material discharge part 160 may be connected to a lower portion of the reaction tank 110, and the vaporized material discharge part 170 may be connected to an upper portion of the reaction tank 110.
[0062] Also, a second control valve 161 may be provided in the liquid material discharge part 160 to control the discharge of the generated liquid material, and a third control valve 171 may be provided in the vaporized material discharge part 170 to control the discharge of the vaporized material such as the vaporized alcohol and water.
[0063] In the sensing process, the liquid-accommodated state in the N partition regions N, N−1, and N−2 may be individually sensed through a sensing unit 140. Here, in the sensing process, the liquid-accommodated state information sensed through the sensing unit 140 may be transmitted to the controller 130.
[0064] In addition, in the sensing process, an accommodated level (height) of a liquid R accommodated in the accommodation part 111 may be sensed through a liquid level sensor disposed inside the reaction tank 110, which is the sensing unit 140.
[0065] In the control process, the heating unit 120 may be controlled through the controller 130 during the heating process so that only the partition regions N, N−1, and N−2, in which the liquid R is accommodated, among the N partition regions N, N−1, and N−2 are heated by the heating unit 120.
[0066] In addition, in the control process, the controller 130 may determine whether the liquid is accommodated in each of the partition regions N, N−1, and N−2 of the accommodation part 111 through sensed accommodation level values of the accommodated liquid R, which are sensed in the sensing process. Here, in the control process, the controller 130 may control the supply of the high-temperature liquid so that the high-temperature liquid is supplied to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain the liquid R, among the N partition regions N, N−1, N−2, and the supply of the high-temperature liquid to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain no liquid R, among the N partition regions N, N−1, N−2 is blocked.
[0067] Furthermore, in the control process, for example, the controller 130 may control opening and closing of a supply part valve V for opening and closing each of the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c to control supply of the high-temperature fluid to the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c. Here, in the control process, particularly, the supply part valve V disposed in each of the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain the liquid R, among the N partition regions N, N−1, N−2 may be opened to supply a high-temperature fluid, and the supply part valve V disposed in each of the heat source supply tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N−1, N−2, which are determined to contain no liquid R, among the N partition regions N, N−1, N−2 may be closed to block the supply of the high-temperature fluid.
[0068] The controller 130 may be connected to the raw material supply part 150 through the first control valve 151, connected to the liquid martial discharge part 160 through the second control valve 161, and connected to the vaporized material discharge part 170 through the third control valve 171 to control the first control valve 151, the second control valve 161, and the third control valve 171. Accordingly, in the control process, a supply amount of raw material, an amount of generated liquid material, and an amount of vaporized material may be controlled through the controller 130. Here, in the control process, the accommodated level (height) of the liquid R accommodated in the accommodation part 111 of the reaction tank 110 may be controlled through the controller 130. Therefore, In the control process, the accommodated level (height) of the liquid R may be controlled through the controller 130 to correspond to an appropriate height of each of the N partition regions N, N−1, and N−2 in the accommodation part 111, which are individually heated by the heat source supply parts 121, 122, and 123.
[0069] While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the scope of the present invention is not limited to the esterification reaction apparatus and the esterification reaction method according to the present invention. It will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention.
[0070] Furthermore, the scope of protection of the present invention will be clarified by the appended claims.
DESCRIPTION OF REFERENCE NUMERALS
[0071] 100: Esterification reaction apparatus [0072] 110: Reaction tank [0073] 111: Accommodation part [0074] 120: heating unit [0075] 121: First heat source supply part [0076] 121a: first heat source supply tube [0077] 121b: Second heat source supply tube [0078] 121c: Third heat source supply tube [0079] 122: Second heat source supply part [0080] 122a: First heat source supply tube [0081] 122b: Second heat source supply tube [0082] 122c: Third heat source supply tube [0083] 123: Third heat source supply part [0084] 123a: First heat source supply tube [0085] 123b: Second heat source supply tube [0086] 123c: Third heat source supply tube [0087] 130: Controller [0088] 140: Sensing unit [0089] 141: First liquid level sensor [0090] 142: Second liquid level sensor [0091] 150: Raw material supply part [0092] 151: First control valve [0093] 160: Liquid material discharge part [0094] 161: Second control valve [0095] 170: Vaporized material discharge part [0096] 171: Third control valve [0097] 180: Stirrer [0098] R: Liquid [0099] V: Supply part valve [0100] V1: First supply part valve [0101] V2: Second supply part valve [0102] V3: Third supply part valve [0103] X; Central axis