阅读说明：本技术 酯化反应装置和酯化反应方法 (Esterification reaction apparatus and esterification reaction method ) 是由 秋渊旭 李成圭 田炯 金显圭 陈赞携 朴振成 于 2020-09-18 设计创作，主要内容包括：本发明涉及一种酯化反应装置及酯化反应方法。根据本发明的酯化反应装置包括：反应槽,形成有用于容纳原料的容纳部,原料包括被供应的羧酸和醇；加热单元,用于独立地加热在容纳部的垂直方向上被划分为N个区域(N是2以上的整数)的每个分隔区域；以及控制器,用于控制加热单元,从而仅加热N个分隔区域中的放置有液体的分隔区域,其中发生原料的酯化反应。(The invention relates to an esterification reaction device and an esterification reaction method. The esterification reaction apparatus according to the present invention comprises: a reaction tank formed with a housing part for housing raw materials including a supplied carboxylic acid and an alcohol; a heating unit for independently heating each of the divided regions divided into N regions (N is an integer of 2 or more) in a vertical direction of the accommodating portion; and a controller for controlling the heating unit so that only the divided regions in which the liquid is placed among the N divided regions, in which the esterification reaction of the raw materials occurs, are heated.)

1. An esterification reaction apparatus comprising:

a reaction tank having a housing portion that houses a raw material containing a carboxylic acid and an alcohol that is supplied therein;

a heating unit configured to independently heat a partition region divided into N regions in a vertical direction of the accommodating part, wherein N is an integer of 2 or more; and

a controller configured to control the heating unit so as to heat only a partition region containing liquid of the N partition regions by controlling the heating unit,

thereby carrying out the esterification reaction of the raw materials.

2. The esterification reaction apparatus according to claim 1, wherein the heating unit includes N heat source supplies respectively provided in the N divided regions.

3. The esterification reaction apparatus according to claim 2, wherein each of the heat source supply portions includes therein a heat source tube in the form of a coil through which a high-temperature fluid as a heat source flows.

4. The esterification reaction apparatus according to claim 3, wherein the heat source supply portion includes a plurality of heat source tubes wound in the form of the coil at different widths around a vertical central axis.

5. The esterification reaction apparatus according to claim 4, wherein the plurality of heat source tubes are provided in a shape wound around the vertical central axis of the housing part in the reaction tank a plurality of times.

6. The esterification reaction apparatus according to any one of claims 3 to 5, wherein the coil pitch of each of the heat source tubes disposed in a lowermost divided region of the N divided regions is equal to or smaller than the coil pitch of each of the heat source tubes disposed in the remaining regions.

7. The esterification reaction apparatus according to claim 3, wherein the high temperature fluid comprises steam.

8. The esterification reaction apparatus according to claim 3, further comprising a sensing unit configured to sense a liquid containing state in the N number of the partitioned areas,

wherein the sensing unit is configured to transmit the sensed information of the liquid containing state to the controller.

9. The esterification reaction apparatus according to claim 8, wherein the sensing unit includes a liquid level sensor provided in the reaction tank to measure a contained height or a liquid level of the liquid contained in the containing portion.

10. The esterification reaction apparatus according to claim 9, wherein the controller is configured to determine whether the liquid is contained in each of the partitioned areas of the containing portion through a liquid level sensing value of the contained liquid sensed by the sensing unit such that the high temperature liquid is supplied to the heat source pipe of the partitioned area of the N partitioned areas determined to contain the liquid and the high temperature liquid is prevented from being supplied to the heat source pipe of the partitioned area of the N partitioned areas determined to not contain the liquid.

11. An esterification reaction process comprising:

a supply step of supplying a raw material containing a carboxylic acid and an alcohol to a housing part of a reaction tank;

a heating step of independently heating, by a heating means, a partition region divided into N regions in a vertical direction of the housing portion, where N is an integer of 2 or more; and

a control step of controlling the heating unit by a controller so that only a partition region containing liquid among the N partition regions is heated,

thereby carrying out the esterification reaction of the raw materials.

12. The esterification reaction method according to claim 11, wherein in the heating process, the partitioned regions of the housing portion are heated by N heat source supply portions constituting the heating unit, which are provided in the N partitioned regions, respectively.

13. The esterification reaction method according to claim 12, wherein in the heating process, the partitioned areas of the housing parts are respectively heated using heat source tubes, each of the heat source tubes is in the form of a coil, and a high-temperature fluid as a heat source flows through the inside of the heat source supply part through each of the heat source tubes.

14. The esterification reaction process according to claim 13, wherein steam is used as the high temperature fluid flowing through the heat source pipe in the heating process.

15. The esterification reaction process according to claim 13, further comprising a sensing process of independently sensing the liquid receiving state in the N number of the partitioned areas by a sensing unit,

wherein, in the sensing process, the information of the liquid containing state sensed by the sensing unit is transmitted to the controller.

16. The esterification reaction method according to claim 15, wherein in the sensing process, a contained height or a liquid level of the liquid contained in the containing section is sensed by a liquid level sensor as the sensing unit and provided in the reaction tank.

17. The esterification reaction method according to claim 16, wherein, in the control process, the controller determines whether the liquid is contained in each of the partitioned areas of the containing part by a liquid level sensing value of the contained liquid sensed by the sensing unit such that the high temperature liquid is supplied to the heat source pipe of the partitioned area determined to contain the liquid among the N partitioned areas and the high temperature liquid is prevented from being supplied to the heat source pipe of the partitioned area determined not to contain the liquid among the N partitioned areas.

Technical Field

Cross Reference to Related Applications

This application claims priority to korean patent application No. 10-2019-0119165, filed on 26.9.2019, the entire contents of which are incorporated herein by reference.

Technical Field

The invention relates to an esterification reaction device and an esterification reaction method.

Background

Phthalate-based plasticizers account for 92% of The global plasticizer market by The 20 th century (see mustaffy lahoman and christoph s. brazel, "plasticizer market: evaluation and trend research on conventional plasticizers to address new challenges (The plasticizer market: an assessment of traditional plasticizers and research trends) and" advanced Polymer Science ", 2004, volume 29, p. 1223-1248). Phthalate-based plasticizers are additives mainly used to impart flexibility, durability, cold resistance to polyvinyl chloride (hereinafter, referred to as PVC), and to reduce viscosity during melting to improve processability. Phthalate-based plasticizers are added to PVC in varying amounts and are widely used in a variety of applications ranging from hard products such as rigid pipes to soft products such as food packaging materials, blood bags, flooring materials, etc. due to their softness and good tensile properties. Therefore, it is more closely linked to real life than any other material, and direct contact with the human body may be unavoidable.

However, although phthalate-based plasticizers have compatibility with PVC and excellent ability to impart flexibility, recently, the following controversy has existed with respect to the harmfulness of PVC products containing phthalate-based plasticizers: when used in real life, Phthalate-based plasticizers may leak from PVC products and act as suspected endocrine disrupters (Environmental hormones) and carcinogens at heavy metal Levels (see NR Janua (N.R. Janjua) et al, "Systemic absorption of Diethyl Phthalate, Dibutyl Phthalate and Butyl Paraben with Systemic Topical Application, Reproductive and Thyroid Hormone Levels in Humans" (systematic upper of dimethyl Phthalate, and Butyl Following the human body), Environmental Science and Technology (Environmental Science and Technology), 2008, Vol. 42, p. 7522-7527). In particular, since the U.S. reported in the 60 th of the 20 th century that the most commonly used phthalate-based plasticizer di (2-ethylhexyl) phthalate, DEHP, was leaked from PVC products, interest in environmental hormones in the 90 th of the 20 th century increased, and global environmental regulations on the harm of phthalate-based plasticizers to human bodies and various studies began to be conducted.

Accordingly, many researchers are conducting research to develop a leakage control technique to suppress leakage of phthalate plasticizers, thereby not only significantly reducing human risks but also meeting environmental standards, as well as to develop a novel non-phthalate-based substitute plasticizer that does not include phthalic anhydride for manufacturing di (2-ethylhexyl) phthalate, or to develop a phthalate plasticizer that can substitute for di (2-ethylhexyl) phthalate and can be used for industrial use because it can suppress leakage of plasticizers even based on phthalate, so as to cope with environmental hormone problems and environmental regulations due to leakage of phthalate plasticizers, particularly di (2-ethylhexyl) phthalate.

As described above, development of di (2-ethylhexyl) phthalate, which has no environmental problems and can replace the existing environmental problems, as a material of a diester-based plasticizer is actively proceeding, and research on development of a diester plasticizer having excellent physical properties and research on equipment for manufacturing such plasticizer are actively proceeding. Here, in terms of process design, more efficient, more economical, and simpler process design is required.

In order to manufacture the above-mentioned diester plasticizer, manufacturing the diester plasticizer includes a reaction process of applying heat to the raw material to perform an esterification reaction, but when a heat source is supplied to the raw material in the reaction process, heat transfer efficiency is low, and the raw material is carbonized to generate foreign substances.

[ Prior Art document ] (patent document) Korean patent laid-open publication No. 10-2019-

Disclosure of Invention

Technical problem

An aspect of the present invention is to provide an esterification reaction apparatus and an esterification reaction method capable of improving heat transfer efficiency and preventing carbonization of raw materials when a heat source is supplied to a receiving part of a reaction tank to supply the heat source to the raw materials to cause an esterification reaction.

Technical scheme

An esterification reaction apparatus comprising: a reaction tank having a housing portion that houses a raw material containing a carboxylic acid and an alcohol that is supplied; a heating unit configured to independently heat a divided region divided into N regions (N is an integer of 2 or more) in a vertical direction of the accommodating portion; and a controller configured to control the heating unit so as to heat only the divided region containing the liquid out of the N divided regions by controlling the heating unit, thereby performing the esterification reaction of the raw materials.

An esterification reaction process comprising: a supply step of supplying a raw material containing a carboxylic acid and an alcohol to a housing part of a reaction tank; a heating step of independently heating, by a heating means, a partition region divided into N regions (N is an integer of 2 or more) in the vertical direction of the housing portion; and a control step of controlling the heating unit by the controller so that only the liquid-containing divided regions of the N divided regions are heated to perform the esterification reaction of the raw materials in the heating step.

Advantageous effects

According to the present invention, it is possible to improve heat transfer efficiency by supplying a heat source only to the wet zone containing the liquid in the accommodating portion of the reaction tank in which the esterification reaction occurs by applying heat to the raw material containing the carboxylic acid and the alcohol. Here, the supply of the heat source to the dry area in which the liquid is not accommodated in the accommodating portion may be prevented to prevent the generation of foreign substances due to carbonization of the raw material provided in the dry area.

Drawings

Fig. 1 is a perspective view of an esterification reaction apparatus according to an embodiment of the present invention.

FIG. 2 is a sectional view of an esterification reaction apparatus according to an embodiment of the present invention.

Fig. 3 is a conceptual sectional view showing an example of an esterification reaction apparatus according to an embodiment of the present invention.

Fig. 4 is a plan view showing an example of the inside of a reaction tank in an esterification reaction apparatus according to an embodiment of the present invention.

Fig. 5 is an exploded perspective view showing an example of a plurality of heat source tubes provided in a heat source supply portion in an esterification reaction device according to an embodiment of the present invention.

Detailed Description

The objects, specific advantages and novel features of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the drawings. It should be noted that the same reference numerals are added to the components of the drawings in the present specification as much as possible even if the reference numerals are shown in other drawings. Furthermore, 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, detailed descriptions of related art that may unnecessarily obscure the gist of the present invention will be omitted.

Fig. 1 is a perspective view of an esterification reaction apparatus according to an embodiment of the present invention. FIG. 2 is a sectional view of an esterification reaction apparatus according to an embodiment of the present invention. Fig. 3 is a conceptual sectional view showing an example of an esterification reaction apparatus according to an embodiment of the present invention.

Fig. 4 is a plan view showing an example of the inside of a reaction tank in an esterification reaction apparatus according to an embodiment of the present invention. Fig. 5 is an exploded perspective view showing an example of a plurality of heat source tubes provided in a heat source supply portion in an esterification reaction device according to an embodiment of the present invention.

Referring to fig. 1 to 3, an esterification reaction apparatus 100 according to an embodiment of the present invention includes a reaction tank 110 in which a receiving part 111 is formed, a heating unit 120 heating partitioned areas N, N-1 and N-2 of the receiving part 111, respectively, and a controller 130 controlling the heating unit 120 to perform an esterification reaction of raw materials. The esterification reaction apparatus 100 according to an embodiment of the present invention may further include a sensing unit 140 for sensing a liquid receiving state.

In more detail, the reaction tank 110 includes a receiving part 111, and raw materials including carboxylic acid and alcohol supplied from the outside are received in the receiving part 111.

Here, the carboxylic acid may include, for example, one or more materials selected from the group consisting of terephthalic acid, phthalic acid, isophthalic acid, and cyclohexane dicarboxylic acid.

Here, the alcohol has 3 to 10 alkyl carbon atoms.

The raw material may be supplied from the outside of the reaction tank 110 to the receiving part 111 of the reaction tank 110 through the raw material supply part 150. Here, the raw material supplied to the receiving part 111 of the reaction tank 110 may be stirred by the stirrer 180 provided in the receiving 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.

The heating unit 120 may heat each of the dividing regions N, N-1 and N-2 divided into N regions (N is an integer of 2 or more) in the vertical direction of the accommodating portion 111, respectively. (although three separate regions are shown in FIG. 3, the number of separate regions in the receiving part of the present invention is not necessarily limited to three.)

In addition, the heating unit 120 may include N heat source supplies 121, 122, and 123 respectively disposed in the N dividing regions N, N-1 and N-2. Here, the heating unit 120 may further include a supply valve V for opening and closing each of the N heat source supplies 121, 122, and 123.

Further, the heating unit 120 may include, for example, a first heat source supply part 121 disposed in an upper portion of the accommodating part 111 in a vertical direction, a second heat source supply part 122 disposed at a central portion of the accommodating part 111, and a third heat source supply part 123 disposed in a lower portion of the accommodating part 111, although the number of the heat source supply parts 121, 122, 123 of the heating unit 120 is not limited thereto. Here, the heating unit 120 may include, for example, a first supply valve V1 for opening and closing the first heat source supply 121, a second supply valve V2 for opening and closing the second heat source supply 122, and a third supply valve V3 for opening and closing the third heat source supply 123.

Referring to fig. 2 to 5, the heat source supply parts 121, 122, 123 may include heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, each of which has the form of a coil through which a high-temperature fluid as a heat source passes. Here, the high-temperature fluid may include steam, for example. Here, a supply valve V for opening and closing each of the heat source supplies 121, 122, and 123 may be installed on each of the heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c in the heat source supplies 121, 122, and 123.

In addition, the heat source supplying parts 121, 122, and 123 may include a plurality of heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c wound in a coil form around the vertical central axis X, having different widths a, b, and c. Here, each of the N heat source supplies 121, 122, and 123 may include a plurality of heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, each of which has the form of a coil. Therefore, the housing 111 of the reaction tank 110 can be uniformly heated. Here, the heat source supply parts 121, 122 and 123 among the N heat source supply parts 121, 122 and 123, which are disposed in the partition regions N, N-1 and N-2 of the receiving part 111 supplying the heat source, may uniformly heat the respective partition regions N, N-1 and N-2.

Further, the plurality of heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may include, for example, first and second heat source tubes 121a, 122a, and 123a, 121b, 122b, and 123b and third heat source tubes 121c, 122c, and 123c arranged in order of having the maximum winding widths a, b, and c. That is, the first heat source tubes 121a, 122a, and 123a each having the maximum winding width a are disposed in a spiral curve shape to be closest to the reaction tank 110, the third heat source tubes 121c, 122c, and 123c each having the minimum winding width c are disposed in a spiral curve shape to be closest to the vertical central axis X of the receiving part 111, and the second heat source tubes 121b, 122b, 123b each having the winding width b between the first heat source tubes 121a, 122a, and 123a and the third heat source tubes 121c, 122c, and 123c are disposed in a spiral curve shape between the first heat source tubes 121a, 122a, and 123a and the third heat source tubes 121c, 122c, and 123 c. However, the number of heat source 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.

In addition, for example, a plurality of heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may be provided in a shape wound around the vertical central axis X of the receiving part 111 in the reaction tank 110 a plurality of times.

In addition, the coil pitch P of each of the heat source tubes 123a, 123b, and 123c disposed in the lowermost partition region N-2 among the N partition regions N, N-1 and N-2 of the accommodating part 111 may be equal to or smaller than the coil pitch P of each of the heat source tubes 121a, 122a, 121b, 122b, 121c, and 122c disposed in the remaining regions N and N-1. Therefore, the heat transfer efficiency in the lowermost partition region N-2 of the containing part 111, which always contains the liquid raw material, can be further improved, thereby improving the reaction efficiency.

The carboxylic acid and alcohol heated by the heating unit 120 cause an esterification reaction to produce an ester-based material and water as a product of the esterification reaction. Here, the ester-based substance in a liquid state may be generated through the esterification reaction and then discharged to the outside of the reaction tank 110 through the liquid substance discharge part 160, and water may be generated, but the water is vaporized to be discharged to the outside of the reaction tank 110 through the vaporized substance discharge part 170.

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.

In addition, a second control valve 161 may be provided in the liquid substance discharge part 160 to control discharge of the generated liquid substance, and a third control valve 171 may be provided in the vaporized substance discharge part 170 to control discharge of the vaporized substance. (see FIG. 1)

Referring to fig. 3, the sensing unit 140 may sense a liquid containing state in the N dividing regions N, N-1 and N-2 of the containing part 111.

In addition, the sensing unit 140 may transmit the sensed liquid containing state information to the controller 130.

Further, the sensing unit 140 may include liquid level sensors 141 and 142 disposed inside the reaction tank 110 to measure a receiving height (liquid level) of the liquid R received in the receiving part 111.

Here, the sensing unit 140 may include a first liquid level sensor 141 disposed in an upper portion of the receiving part 111 of the reaction tank 110 and a second liquid level sensor 142 disposed in a lower portion of the receiving part 111 of the reaction tank 110.

Referring to fig. 1 and 3, the controller 130 may control the heating unit 120 to heat only the N divided regions N, N-1 and N-2 in which the liquid R is disposed in the divided regions N, N-1 and N-2. Here, the controller 130 may control the supply portion valve V for opening and closing each of the N heat source supply portions 121, 122 and 123 to control the supply of the heat source of the heating unit 120.

In addition, the controller 130 may determine whether liquid is contained in each of the divided regions N, N-1 and N-2 of the containing part 111 through a liquid level sensing value of the contained liquid R sensed by the sensing unit 140. Here, the controller 130 may control the supply of the high temperature liquid such that the high temperature liquid is supplied to the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined to contain the liquid R among the N partition regions N, N-1, N-2, and prevent the high temperature liquid from being supplied to the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined not to contain the liquid R among the N partition regions N, N-1, N-2.

Here, the dividing regions N, N-1 and N-2 heated by supplying the high-temperature fluid to the heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may be heated at a temperature of 150 ℃ to 230 ℃, for example. Here, in particular, the dividing regions N, N-1 and N-2 heated by supplying a high-temperature fluid to the heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c may be heated at a temperature of 180 ℃, for example. Here, the opening and closing of each of the supply valves V1, V2, and V3 may be controlled by the controller 130 so that the respective partition regions N, N-1 and N-2 are heated by the heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c constituting the heating unit 120, respectively.

The controller 130 may be connected to the raw material supply part 150 through a first control valve 151, to the liquid substance discharge part 160 through a second control valve 161, and to the vaporized substance discharge part 170 through a third control valve 171 to control the first control valve 151, the second control valve 161, and the third control valve 171. (here, since a technique of electrically controlling a valve by a controller is a well-known technique, a description of an operation principle and a control principle of the valve will be omitted)

Referring to fig. 1 to 3, in an esterification reaction apparatus 100 including the above-described members, according to an embodiment of the present invention, a receiving part 111 of a reaction tank 110 may be divided into N regions where heat is applied to raw materials including carboxylic acid and alcohol to cause an esterification reaction. And the divided regions N, N-1 and N-2 may be heated by the heating unit 120, respectively. Here, the controller may control the heating unit 120 such that only the divided regions N, N-1 and N-2 containing the liquid R are heated.

Therefore, the heat source may be supplied only to the wet areas containing the liquid R in the N dividing regions N, N-1 and N-2 of the container 111 to significantly improve the heat transfer efficiency. That is, when heat is applied to the raw material mixed with liquid carboxylic acid and alcohol to cause the esterification reaction, only a region containing the raw material solution mixed with carboxylic acid and alcohol to cause the esterification reaction may be heated to prevent a problem that a heat source is unnecessarily applied to a region not containing the raw material solution without causing the esterification reaction to lower efficiency.

In addition, the supply of the heat source to the dry region not containing the liquid R can be inhibited to prevent carbonization of the raw material. That is, when heat is applied to a raw material mixed with a liquid carboxylic acid and an alcohol to cause an esterification reaction, it is possible to prevent the problem of foreign substances being generated by carbonization of a solid or gaseous material by applying heat to the solid or gaseous material in the raw material by blocking the supply of a heat source to a dry zone.

Hereinafter, an esterification reaction method according to an embodiment of the present invention will be described.

Referring to fig. 1 to 3, an esterification reaction method according to an embodiment of the present invention includes: a supply step of supplying the raw material to the accommodating portion 111 of the reaction tank 110; a heating step of heating the divided regions N, N-1 and N-2 of the accommodating section 111; and a control step of controlling the heating unit 120 by the controller to perform the esterification reaction in the heating step. In addition, the esterification reaction method according to an embodiment of the present invention may further include a sensing process of sensing a liquid receiving state.

More specifically, in the supply step, the raw material containing the carboxylic acid and the alcohol may be supplied to the housing portion 111 of the reaction tank 110.

In the supply step, for example, the liquid carboxylic acid and the alcohol may be mixed and supplied to the housing portion 111 of the reaction tank 110 through the raw material supply portion 150. Here, a first control valve 151 is provided in the raw material supply part 150 to control the supply of the raw material.

The carboxylic acid may include, for example, one or more materials selected from the group consisting of terephthalic acid, phthalic acid, isophthalic acid, and cyclohexane dicarboxylic acid.

The alcohol may have 3 to 10 alkyl carbon atoms.

In the supply step, the molar ratio of the amount of carboxylic acid added to the housing 111 of the reaction tank 110 to the total amount of primary alcohol added may be, for example, 1:2 to 1: 5.

In the heating process, the partition regions N, N-1 and N-2 divided into N regions (N is an integer of 2 or more) in the vertical direction of the accommodating portion 111 may be heated by the heating unit 120, respectively.

In addition, in the heating process, the partition regions N, N-1 and N-2 of the accommodating part 111 may be heated by the N heat source supplying parts 121, 122 and 123 constituting the heating unit 120, which are respectively disposed in the N partition regions N, N-1 and N-2.

Further, the divided regions N, N-1 and N-2 of the container part 111 may be heated using heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c, respectively, each of which has a coil form and through which a high-temperature fluid as a heat source passes through the inside of the heat source supply parts 121, 122, and 123.

In addition, in the heating process, steam may be used as a high temperature fluid passing through the heat source tubes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123 c.

The carboxylic acid and alcohol may be subjected to an esterification reaction by a heating process to produce an ester-based material and water as the esterification reaction product.

Here, the liquid ester-based substance generated through the esterification reaction may be discharged to the outside of the reaction tank 110 through the liquid substance discharge part 160, and water may be vaporized to be discharged to the outside of the reaction tank 110 through the vaporized substance discharge part 170.

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.

In addition, a second control valve 161 may be provided in the liquid material discharge part 160 to control discharge of the generated liquid material, and a third control valve 171 may be provided in the vaporized material discharge part 170 to control discharge of the vaporized material (e.g., vaporized ethanol and water).

In the sensing process, the liquid containing states in the N partition regions N, N-1 and N-2 may be sensed by the sensing unit 140, respectively. Here, in the sensing process, the liquid receiving state information sensed by the sensing unit 140 may be transmitted to the controller 130.

In the sensing step, the storage height (level) of the liquid R stored in the storage section 111 may be sensed by a level sensor as the sensing unit 140 provided in the reaction tank 110.

In the control process, the heating unit 120 may be controlled by the controller 130 in the heating process such that only the partition regions N, N-1 and N-2 containing the liquid R among the N partition regions N, N-1 and N-2 are heated by the heating unit 120.

In addition, in the control process, the controller 130 may determine whether liquid is contained in each of the divided regions N, N-1 and N-2 of the containing part 111 by a liquid level sensing value of the contained liquid R sensed in the sensing process. Here, in the control process, the controller 130 may control the supply of the high temperature liquid such that the high temperature liquid is supplied to the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined to contain the liquid R among the N partition regions N, N-1, N-2, and the high temperature liquid is prevented from being supplied to the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined not to contain the liquid R among the N partition regions N, N-1, N-2.

Further, in the control process, for example, the controller 130 may control the opening and closing of the supply valve V for opening and closing each of the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c to control the supply of the high-temperature fluid to the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123 c. Here, in the control process, specifically, the supply portion valve V provided in each of the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined to contain the liquid R among the N partition regions N, N-1, N-2 may be opened to supply the high temperature fluid, and the supply portion valve V provided in each of the heat source pipes 121a, 122a, 123a, 121b, 122b, 123b, 121c, 122c, and 123c of the partition regions N, N-1, N-2 determined not to contain the liquid R among the N partition regions N, N-1, N-2 may be closed to prevent the supply of the high temperature fluid.

The controller 130 may be connected to the raw material supply part 150 through a first control valve 151, to the liquid substance discharge part 160 through a second control valve 161, and to the vaporized substance discharge part 170 through a third control valve 171 to control the first control valve 151, the second control valve 161, and the third control valve 171. Therefore, in the control process, the supply amount of the raw material, the amount of the liquid material produced, and the amount of the vaporized material can be controlled by the controller 130. Here, in the control step, the storage height (level) of the liquid R stored in the storage section 111 of the reaction tank 110 may be controlled by the controller 130. Therefore, in the control process, the containing height (level) of the liquid R may be controlled by the controller 130 to correspond to an appropriate height of each of the N divided regions N, N-1 and N-2 in the containing part 111 that are heated by the heat source supply parts 121, 122, and 123, respectively.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it should be understood that the scope of the present invention is not limited to esterification reaction apparatuses and esterification reaction processes 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.

Furthermore, the scope of the invention is set forth in the appended claims.

[ description of reference numerals ]

100: esterification reaction device

110: reaction tank

111: accommodating part

120: heating unit

121: a first heat source supply part

121 a: first heat source tube

121 b: second heat source tube

121 c: third heat source tube

122: second heat source supply part

122 a: first heat source tube

122 b: second heat source tube

122 c: third heat source tube

123: third heat source supply part

123 a: first heat source tube

123 b: second heat source tube

123 c: third heat source tube

130: controller

140: sensing unit

141: first liquid level sensor

142: second liquid level sensor

150: raw material supply part

151: first control valve

160: liquid substance discharge part

161: second control valve

170: vaporized material discharge part

171: third control valve

180: stirrer

R: liquid, method for producing the same and use thereof

V: supply part valve

V1: first supply part valve

V2: second supply part valve

V3: third supply part valve

X: center shaft