Neutralization / water separation tank for esterification products and method for neutralizing / separating esterification products

Abstract

An esterification product neutralization / water separation tank according to an embodiment of the present invention for solving the above problems includes: a neutralization section into which an unrefined product mixture containing an alcohol and an ester compound, a neutralizing agent, and water are introduced to form a neutralized mixture; a water separation section that separates the neutralized mixture into a floating layer and an aqueous layer; a first partition wall extending upward from the bottom to form an upper passage and separating the neutralization section from the water separation section; and a second partition wall extending downward from the ceiling to form a lower passage, wherein the water separation section includes the first water separation section into which the neutralized mixture flows from the neutralization section through the upper passage; and a second water separation section into which the neutralized mixture flows from the first water separation section through the lower passage, and the first water separation section and the second water separation section are separated by the second partition wall.

Description

Technical Field

[0001] [Cross - reference to Related Applications] This application claims the benefit of priority based on Korean Patent Application No. 10 - 2019 - 0115693, filed on September 19, 2019, and all the contents disclosed in the literature of the Korean patent application are incorporated herein by reference in their entirety.

[0002] The present invention relates to a neutralization / water separation tank for esterification products and a method for neutralizing / water - separating esterification products. More specifically, it relates to a neutralization / water separation tank for esterification products and a method for neutralizing / water - separating esterification products in which both neutralization reaction and water separation occur well during the production of plasticizers, and the efficiency can be increased.

Background Art

[0003] Phthalate plasticizers accounted for 92% of the world's plasticizer market until the 20th century (see Mustafizur Rahman and Christopher S. Brazel, "The plasticizer market: an assessment of traditional plasticizers and research trends to meet new challenges", Progress in Polymer Science 2004, 29, 1223 - 1248). They are additives mainly used to impart flexibility, durability, cold resistance, etc. to polyvinyl chloride (hereinafter referred to as PVC), lower the viscosity during melting to improve processability, and are added to PVC in various contents. They have a closer relationship with real life than any other material, ranging from hard products such as hard pipes to soft products that can be used for food packaging materials, blood bags, floor materials, etc., which are widely used in applications where direct contact with the human body is inevitable.

[0004] However, despite the compatibility of phthalate plasticizers with PVC and their excellent softening properties, recent concerns have been raised about the potential harmful effects of phthalate plasticizers on PVC products used in everyday life. These plasticizers may leach out into the product over time, potentially acting as endocrine disruptors (environmental hormones) and carcinogens at heavy metal levels (see NRJanjua et al. "Systemic Uptake of Diethyl Phthalate, Dibutyl Phthalate, and Butyl Paraben Following Whole-body Topical Application and Reproductive and Thyroid Hormone Levels in Humans," Environmental Science and Technology 2008, 42, 7522-7527). In particular, after reports were published in the United States in the 1960s that diethylhexyl phthalate (DEHP), the most widely used phthalate plasticizer, was leaking into PVC products, interest in endocrine disruptors increased in the 1990s. This led to a variety of studies on the harmful effects of phthalate plasticizers on the human body, as well as the implementation of global environmental regulations.

[0005] Therefore, many researchers are working to address the problem of endocrine disruptors caused by the leaching of phthalate-based plasticizers and to comply with environmental regulations. This involves either developing new non-phthalate alternative plasticizers that eliminate phthalic anhydride, which is used in the manufacture of phthalate-based plasticizers, or developing leaching control technologies that not only significantly reduce the harm to human health by suppressing the leaching of phthalate-based plasticizers but also comply with environmental standards.

[0006] On the other hand, terephthalate-based plasticizers, as non-phthalate plasticizers, are attracting attention not only because they are at the same level as phthalate-based plasticizers in terms of physical properties, but also because they do not cause environmental problems. In fact, various types of terephthalate-based plasticizers are being developed, and research is actively progressing not only on developing terephthalate-based plasticizers with superior physical properties, but also on research on equipment for manufacturing such terephthalate-based plasticizers. From the perspective of process design, there is a demand for more efficient, economical, and simpler process designs. [Overview of the project] [Problems that the invention aims to solve]

[0007] The problem that the present invention aims to solve is to provide a neutralization / water separation tank for esterification products and a method for neutralizing / separating esterification products that can increase efficiency by ensuring that both the neutralization reaction and water separation occur well when producing plasticizers.

[0008] The problems addressed by the present invention are not limited to those mentioned above, and other problems not mentioned can be clearly understood by those skilled in the art from the following description. [Means for solving the problem]

[0009] A neutralization / water separation tank for esterification products according to an embodiment of the present invention for solving the aforementioned problems includes: a neutralization section into which an unrefined product mixture containing alcohol and an ester compound, a neutralizing agent, and water are introduced to form a neutralization mixture; a water separation section for fractionating the neutralization mixture into a floating layer and an aqueous layer; a first partition wall extending upward from the bottom to form an upper passage and separating the neutralization section and the water separation section; and a second partition wall extending downward from the ceiling to form a lower passage, wherein the water separation section includes a first water separation section into which the neutralization mixture flows in from the neutralization section via the upper passage; and a second water separation section into which the neutralization mixture flows in from the first water separation section via the lower passage, and the first water separation section and the second water separation section are separated by the second partition wall.

[0010] The system may further include a first discharge pump that discharges the resulting material contained in the suspended layer to the outside from the side wall of the second water separation section.

[0011] The system may further include a second discharge pump that discharges the salt contained in the aqueous layer and settled to the outside from the bottom surface of the water separation unit.

[0012] The system may further include a circulation pump that discharges the neutralized mixture from the neutralization section and reintroduces the neutralized mixture to the neutralization section.

[0013] The system may further include a propeller agitator installed in the neutralization section for stirring the neutralized mixture.

[0014] Furthermore, the bottom surface of the water separation section may be formed to slope downwards as it approaches the center.

[0015] Furthermore, the inclination may be between 5 and 45 degrees.

[0016] Furthermore, the bottom surface of the neutralizing section may be formed to be inclined downwards as it approaches the center.

[0017] Furthermore, the upper passage may have a height of 10 to 50% of the height of the first partition wall.

[0018] Furthermore, the lower passage may have a height of 10 to 50% of the height of the second partition wall.

[0019] A neutralization / water separation method for esterification products according to an embodiment of the present invention for solving the aforementioned problems includes the steps of: introducing an unrefined product mixture containing an alcohol and an ester compound, a neutralizing agent, and water into the neutralization section of a neutralization / water separation tank; mixing the unrefined product mixture, the neutralizing agent, and the water to form a neutralization mixture; allowing the neutralization mixture to flow into a first water separation section of the water separation section via an upper passage; allowing the neutralization mixture to flow into a second water separation section of the water separation section via a lower passage; fractionating the neutralization mixture into a floating layer and a water layer; and discharging the resulting product contained in the floating layer to the outside.

[0020] Also, in the step of forming the neutralization mixture, the circulation pump may discharge the neutralization mixture from the neutralization section and then input the neutralization mixture into the neutralization section again.

[0021] Also, in the step of forming the neutralization mixture, the neutralization mixture may be stirred using a propeller stirrer.

[0022] Also, the bottom surface of the water separation section may be formed to slope downward toward the center, and the salt contained and precipitated in the aqueous layer may gather at the center of the bottom surface of the water separation section.

[0023] Other specific matters of the present invention are included in the detailed description and the drawings.

Advantages of the Invention

[0024] According to an embodiment of the present invention, there are at least the following effects.

[0025] Since the neutralization section where the neutralization reaction occurs and the water separation section where the water separation occurs are formed separately, both the neutralization reaction and the water separation can occur well, and the efficiency can be increased.

[0026] Also, since the neutralization section and the water separation section are integrally formed in one neutralization / water separation tank, a separate transfer pump is not required, so the total volume does not increase, the structure becomes simple, and the problem of salt accumulation can be prevented.

[0027] The effects according to the present invention are not limited to the contents exemplified above, and various other effects are included in this specification.

Brief Description of the Drawings

[0028] [Figure 1] It is a schematic view of a conventional integrated neutralization / water separation tank in which both neutralization and water separation occur. [Figure 2]This is a schematic diagram of a neutralization / water separation device formed by separating a conventional neutralization tank and water separation tank. [Figure 3] This is a schematic diagram of a neutralization / water separation tank according to the first embodiment of the present invention. [Figure 4] This is a schematic diagram of a neutralization / water separation tank according to a second embodiment of the present invention. [Figure 5] This is a schematic diagram of a neutralization / water separation tank according to a third embodiment of the present invention. [Figure 6] This is a schematic diagram of a neutralization / water separation tank according to a fourth embodiment of the present invention. [Modes for carrying out the invention]

[0029] The advantages and features of the present invention, and methods for achieving them, will become apparent with reference to the embodiments described below in detail, along with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below and can be embodied in a variety of different forms, and these embodiments are provided merely to complete the disclosure of the present invention and to fully inform those ordinary skill in the art of the present invention of the scope of the invention, and the present invention is defined only by the scope of the claims. Throughout the specification, the same reference numerals refer to the same components.

[0030] Unless otherwise defined, all terms used herein (including technical and scientific terms) may be used in a way that can be commonly understood by a person of ordinary skill in the art to which the present invention pertains. Furthermore, terms defined in commonly used dictionaries shall not be interpreted ideally or excessively unless explicitly defined otherwise.

[0031] The terms used herein are for illustrative purposes only and are not intended to limit the invention. In this specification, the singular form includes the plural form unless otherwise specified. The terms “comprises” and / or “comprising” as used in this specification do not preclude the presence or addition of one or more other components beyond those mentioned.

[0032] Preferred embodiments of the present invention will be described in detail below with reference to the attached drawings.

[0033] Figure 1 is a schematic diagram of a conventional neutralization / water separation tank 3, which is formed as a single, integrated unit where both neutralization and water separation occur.

[0034] The production of plasticizers involves several main steps: mixing, neutralization, water separation, purification, and filtration. In the mixing step, a carboxylic acid and an alcohol are mixed to undergo an esterification reaction, forming an unrefined product mixture containing the alcohol and the ester compound. In the neutralization step, the unrefined product mixture is neutralized by mixing it with a neutralizing agent, which is a basic aqueous solution. In the water separation step, the neutralized mixture is fractionated into a suspended layer 22 containing organic matter and an aqueous layer 23 containing salt 24. In the purification step, the product is discharged from the suspended layer 22, and any remaining alcohol is removed. In the filtration step, the product is filtered to obtain the final product, the plasticizer.

[0035] In these various stages, the conventional neutralization and water separation method was carried out in a single, integrated container-shaped neutralization / water separation tank 3, as shown in Figure 1. The neutralization / water separation tank 3 is divided into a first space 31 and a second space 32 by a partition wall 33. The partition wall 33 extends upward from the bottom surface 34 of the neutralization / water separation tank 3, forming an upper passage 331.

[0036] First, the unrefined product mixture was introduced into the first space 31 of the neutralization / water separation tank 3 via the first inlet 351, and the neutralizing agent, which is a basic aqueous solution, and water were also introduced into the first space 31 via the second inlet 352. Then, the circulation pump 36 connected to the first space 31 was activated to mix and neutralize the unrefined product mixture, the neutralizing agent, and water, thereby producing a neutralized mixture 21. This mixture was then immediately fractionated into a floating layer 22 containing organic matter and an aqueous layer 23 containing salt 24. When the water level of this neutralized mixture 21 rose above the partition wall 33, the floating layer 22 overflowed and flowed into the second space 32 via the upper passage 331 located above the partition wall 33. Then, the first discharge pump 371 connected to the second space 32 discharged the resulting material from the floating layer 22 to the outside. On the other hand, the salt 24 that settles in the first space 31 does not flow into the second space 32 via the upper passage 331, but settles at the bottom of the first space 31. The second discharge pump 372, which is connected to the first space 31, discharges the settled salt 24 from the aqueous layer 23 to the outside.

[0037] However, the more energy is applied to the neutralization mixture 21 in the first space 31 from the outside to cause it to flow rapidly, the better the neutralization reaction occurs. Conversely, the more energy is left to stand without applying external energy to the neutralization mixture 21, the better the water separation occurs. In other words, the conditions for good neutralization and good water separation are contradictory, so if neither the neutralization reaction nor the water separation occurs well, there is a problem of reduced efficiency.

[0038] Figure 2 is a schematic diagram of the neutralization / water separation device 3a formed by separating the conventional neutralization tank 31a and water separation tank 32a.

[0039] To solve the aforementioned problem, the neutralization tank 31a and the water separation tank 32a were separated separately, as shown in Figure 2. Specifically, the unrefined product mixture was introduced into the neutralization tank 31a of the neutralization / water separation device 3a via the first inlet 351a, and the neutralizing agent, which is a basic aqueous solution, and water were also introduced into the neutralization tank 31a via the second inlet 352a. Then, the circulation pump 36a connected to the neutralization tank 31a was activated to mix and neutralize the unrefined product mixture, the neutralizing agent, and water, thereby producing a neutralized mixture 21. The neutralized mixture 21 was then transferred to the water separation tank 32a using the transfer pump 38. The water separation tank 32a is divided into a first space 321 and a second space 322 by a partition wall 33a. The partition wall 33a extends upward from the bottom surface 34a of the water separation tank, forming an upper passage 331a.

[0040] When the neutralization mixture 21 was introduced into the first space 321 via the transfer pump 38, it was immediately fractionated into a floating layer 22 containing organic matter and an aqueous layer 23 containing salt 24. When the water level of the neutralization mixture 21 rose above the partition wall 33a, the floating layer 22 overflowed through the upper passage 331a located above the partition wall 33a and flowed into the second space 322. The first discharge pump 171, connected to the second space 322, then discharged the resulting material from the floating layer 22 to the outside. Meanwhile, the second discharge pump 172, connected to the first space 321, discharged the precipitated salt 24 from the aqueous layer 23 to the outside. As a result, in the neutralization tank 31a, the neutralization reaction occurred smoothly by applying energy from the outside to the neutralization mixture 21, and in the water separation tank 32a, water separation occurred smoothly by leaving the neutralization mixture 21 without applying energy from the outside, thus increasing efficiency.

[0041] However, such a neutralization / water separation device 3a requires a separate transfer pump 38, which increases the total volume and complicates the structure. Furthermore, when the neutralization / water separation device 3a stops operating, the neutralization mixture 21 may remain in the transfer pump 38, causing the salt 24 to precipitate. When such salt 24 accumulates in the transfer pump, the pressure inside the transfer pump increases, leading to problems with the pump's efficiency and lifespan.

[0042] Figure 3 is a schematic diagram of a neutralization / water separation tank 1 according to the first embodiment of the present invention.

[0043] According to the first embodiment of the present invention, since the neutralization section 11 where the neutralization reaction occurs and the water separation section 12 where water separation occurs are formed separately, both the neutralization reaction and water separation occur well, and efficiency can be increased. Furthermore, since the neutralization section 11 and the water separation section 12 are integrated into a single neutralization / water separation tank 1, a separate transfer pump is not required, so the total volume does not increase, the structure is simplified, and the problem of salt 24 accumulation can be prevented.

[0044] For this purpose, the esterification product neutralization / water separation tank 1 according to one embodiment of the present invention includes: a neutralization section 11 into which an unrefined product mixture containing alcohol and an ester compound, a neutralizing agent, and water are introduced to form a neutralization mixture 21; a water separation section 12 that fractionates the neutralization mixture 21 into a floating layer 22 and a water layer 23; a first partition wall 131 that extends upward from the bottom surface 14 to form an upper passage 1311 and separates the neutralization section 11 and the water separation section 12; and a section extending downward from the ceiling 14a. The water separation section 12 includes a second partition wall 132 which is extended and forms a lower passage 1321 in the water separation section 12, the water separation section 12 includes a first water separation section 121 into which the neutralization mixture 21 flows from the neutralization section 11 via the upper passage 1311, and a second water separation section 122 into which the neutralization mixture 21 flows from the first water separation section 121 via the lower passage 1321, the first water separation section 121 and the second water separation section 122 are separated by the second partition wall 132.

[0045] As mentioned above, the production of plasticizers first involves a mixing step. In this mixing step, a carboxylic acid and an alcohol are mixed, and when an esterification reaction occurs, an unrefined product mixture containing the alcohol and the ester compound is formed.

[0046] Here, the carboxylic acid may be an alkyl carboxylic acid having 2 to 24 carbon atoms, a cycloalkyl carboxylic acid having 3 to 24 carbon atoms, an aromatic carboxylic acid having 6 to 24 carbon atoms, or a mixture thereof. For example, it may be selected from caprylic acid, caproic acid, lauric acid, octanoic acid, decanoic acid, dodecanoic acid, ethaneic acid (acetic acid), propionic acid, butyric acid, pentanoic acid, hexanoic acid, ethylhexanoic acid, cyclohexanecarboxylic acid, benzoic acid, cyclohexane 1,2-dicarboxylic acid, cyclohexane 1,3-dicarboxylic acid, cyclohexane 1,4-dicarboxylic acid, terephthalic acid, isophthalic acid, phthalic acid, or a combination thereof. Preferably, it may be cyclohexane 1,2-dicarboxylic acid, cyclohexane 1,3-dicarboxylic acid, cyclohexane 1,4-dicarboxylic acid, terephthalic acid, isophthalic acid, phthalic acid, or a combination thereof, but it is not necessarily limited to these.

[0047] The alcohol may be an aliphatic alcohol having a C1-C20 alkyl group, preferably an aliphatic primary alcohol having a C3-C10 alkyl group, where the alcohol may have a linear or branched alkyl group, may be a mixed alcohol between structural isomers, and may contain a mixture of alcohols with different numbers of carbon atoms.

[0048] The esterification reaction between an alcohol component and a carboxylic acid may be carried out in the presence of a catalyst. The catalyst may be one or more catalysts commonly used in alcohol esterification reactions, such as acid catalysts like sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, p-toluenesulfonic acid, methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, butanesulfonic acid, and alkylsulfuric acid; metal salts like aluminum lactate, lithium fluoride, potassium chloride, cesium chloride, calcium chloride, iron chloride, and aluminum phosphate; metal oxides like heteropoly acids; natural / synthetic zeolites; cation and anion exchange resins; and organometallic compounds such as tetraalkyl titanates and their polymers.

[0049] Next, the unpurified product mixture undergoes a neutralization step in which it is neutralized with a basic neutralizing agent, and a water separation step in which it is fractionated into a floating layer 22 and an aqueous layer 23. The neutralization / water separation method of the esterification product according to the first embodiment of the present invention is carried out in a single integrated container-shaped neutralization / water separation tank 1, as shown in Figure 3. The neutralization / water separation tank 1 is then separated internally into a neutralization section 11 and a water separation section 12 by a first partition wall 131.

[0050] The neutralization section 11 is a space into which an unrefined product mixture containing an alcohol and an ester compound, a neutralizing agent, and water are introduced to form a neutralized mixture 21. A circulation pump 16 can be connected to such a neutralization section 11, as shown in Figure 3, to discharge the neutralized mixture 21 from the neutralization section 11 and reintroduce the neutralized mixture 21 into the neutralization section 11. When such a circulation pump 16 is in operation, the neutralized mixture 21 can be rapidly and uniformly stirred and neutralized.

[0051] The water separation section 12 is a space that contains the neutralization mixture 21 and divides it into a floating layer 22 and an aqueous layer 23. Here, the floating layer 22 is the part that contains organic matter which later becomes a plasticizer, and the aqueous layer 23 is the part that contains water and salt 24 calculated by the neutralization reaction.

[0052] The first partition wall 131 separates the neutralization section 11 from the water separation section 12. This allows for more efficient neutralization and water separation by applying external energy only to the neutralization section 11. The first partition wall 131 extends upward from the bottom surface 14 of the neutralization / water separation tank 1, forming an upper passage 1311 above it. That is, the neutralization section 11 and the water separation section 12 are not completely isolated by the first partition wall 131, but are connected to each other via the upper passage 1311. Therefore, when the water level of the neutralized mixture 21 neutralized in the neutralization section 11 rises above the first partition wall 131, the neutralized mixture 21 overflows through the upper passage 1311 located above the first partition wall 131 and flows into the water separation section 12.

[0053] On the other hand, it is preferable that the upper passage 1311 has a height of 10 to 50% of the height of the first partition wall 131. If the upper passage 1311 has a height of less than 10% of the height of the first partition wall 131, the unrefined product mixture, neutralizing agent, and water may be added in excessive amounts to cause the neutralization mixture 21 to overflow. And if the upper passage 1311 has a height of more than 50% of the height of the first partition wall 131, the mixture may immediately flow into the water separation section 12 before the neutralization reaction can be completed.

[0054] The water separation section 12 is separated internally into a first water separation section 121 and a second water separation section 122 by a second partition wall 132. The first water separation section 121 is a space that separates the neutralization section 11 and the second water separation section 122. The second water separation section 122 is a space that contains the neutralization mixture 21 and divides it into a floating layer 22 and an aqueous layer 23. The neutralization mixture 21 has a large kinetic energy and flows from the neutralization section 11 to the first water separation section 121 via the upper passage 1311. Then, the neutralization mixture 21 flows from the first water separation section 121 to the second water separation section 122 via the lower passage 1321. Here, because the first water separation section 121 separates the neutralization section 11 and the second water separation section 122, the kinetic energy of the neutralization mixture 21 decreases in the second water separation section 122. Therefore, the water separation of the neutralization mixture 21 occurs well, and it can be further and more rapidly and clearly fractionated into the floating layer 22 and the aqueous layer 23.

[0055] The second partition wall 132 separates the first water separation section 121 from the second water separation section 122. This significantly reduces the kinetic energy when the neutralization mixture 21 is introduced into the second water separation section 122, allowing for more efficient water separation. The second partition wall 132 extends downward from the ceiling 14a of the neutralization / water separation tank 1, forming a lower passage 1321 below it. That is, the first water separation section 121 and the second water separation section 122 are not completely isolated by the second partition wall 132, but are connected to each other via the lower passage 1321. Therefore, the neutralization mixture 21 introduced into the first water separation section 121 flows naturally into the second water separation section 122 via the lower passage 1321 located below the second partition wall 132.

[0056] On the other hand, it is preferable that the lower passage 1321 has a height of 10 to 50% of the height of the second partition wall 132. If the lower passage 1321 has a height lower than 10% of the height of the second partition wall 132, the flow rate of the neutralization mixture 21 will decrease significantly, and the total process time may become excessive. Furthermore, if the lower passage 1321 has a height higher than 50% of the height of the second partition wall 132, the first water separation section 121 will not sufficiently separate the neutralization section 11 and the second water separation section 122, and the kinetic energy of the neutralization mixture 21 flowing into the second water separation section 122 will not decrease significantly, which may reduce the efficiency of water separation.

[0057] On the other hand, a first discharge pump 171 for discharging the resulting material contained in the floating layer 22 to the outside may be connected to the side wall of the second water separation unit 122. Such a first discharge pump 171 is connected from the side wall of the second water separation unit 122 to a height corresponding to the position in which the floating layer 22 floats. The position in which the floating layer 22 floats can also be easily adjusted by adjusting the input amount of unrefined product mixture, neutralizing agent, and water that is input into the first inlet 151 and the second inlet 152, and the output amount of the resulting material discharged by the first discharge pump 171. That is, increasing the input amount or decreasing the output amount raises the floating position of the floating layer 22, and decreasing the input amount or increasing the output amount lowers the floating position of the floating layer 22. However, it is preferable that the floating layer 22 floats at least higher than the position of the lower passage 1321, so the first discharge pump 171 may be connected to a position higher than the lower passage 1321.

[0058] On the other hand, a second discharge pump 172 may be connected to the bottom surface 14 of the water separation unit 12 to discharge the salt 24 contained in the aqueous layer 23 to the outside. As the neutralization mixture 21 flows through the first water separation unit 121 and the second water separation unit 122, it is fractionated into a floating layer 22 and an aqueous layer 23, and the salt 24 contained in the aqueous layer 23 may settle at the bottom of the water separation unit 12. The salt 24 is a compound in which an acidic anion and a basic cation are produced when the unrefined product mixture is neutralized by a neutralizing agent. Therefore, the second discharge pump 172 is connected in particular to the bottom surface 14 of the second water separation unit 122 to discharge the salt 24 settled from the aqueous layer 23 to the outside.

[0059] A method for neutralizing and separating esterification products according to one embodiment of the present invention includes the steps of: introducing an unrefined product mixture containing an alcohol and an ester compound, a neutralizing agent, and water into a neutralization section 11 of a neutralization / water separation tank 1; mixing the unrefined product mixture, the neutralizing agent, and the water to form a neutralization mixture 21; allowing the neutralization mixture 21 to flow into a first water separation section 121 of a water separation section 12 via an upper passage 1311; allowing the neutralization mixture 21 to flow into a second water separation section 122 of a water separation section 12 via a lower passage 1321; fractionating the neutralization mixture 21 into a floating layer 22 and a water layer 23; and discharging the resulting product contained in the floating layer 22 to the outside.

[0060] Specifically, first, an unrefined product mixture containing alcohol and an ester compound is introduced into the neutralization section 11 of the neutralization / water separation tank 1 via the first inlet 151, and a neutralizing agent, which is a basic aqueous solution, and water are also introduced into the neutralization tank via the second inlet 152. Then, the unrefined product mixture, the neutralizing agent, and water are mixed and neutralized to produce a neutralized mixture 21. The neutralizing agent may be an aqueous solution of a basic substance such as an alkali metal hydroxide, an alkaline earth metal hydroxide, or a mixture thereof, for example, an aqueous solution of NaOH or an aqueous solution of KOH may be used.

[0061] Then, the circulation pump 16 connected to the neutralization unit 11 is activated. This circulation pump 16 discharges the neutralization mixture 21 from the neutralization unit 11 and reintroduces the neutralization mixture 21 into the neutralization unit 11. Therefore, the neutralization mixture 21 can be neutralized quickly and uniformly.

[0062] The unrefined product mixture may be introduced into the neutralization tank separately via the first inlet 151, and the neutralizing agent and water via the second inlet 152. However, as shown in Figure 3, the first inlet 151 and the second inlet 152 may be connected in between. In this case, the unrefined product mixture, neutralizing agent, and water may be pre-mixed before being introduced into the neutralization tank and then introduced into the tank via the third inlet 153. This allows for more rapid and uniform neutralization than if the circulation pump 16 were to neutralize the neutralization mixture 21 alone afterward.

[0063] When the neutralized mixture 21, neutralized in the neutralization section 11, rises above the first partition wall 131, the neutralized mixture 21 overflows through the upper passage 1311 located above the first partition wall 131 and flows into the water separation section 12, particularly the first water separation section 121. The neutralized mixture 21 introduced into the first water separation section 121 then naturally flows into the second water separation section 122 through the lower passage 1321 located below the second partition wall 132.

[0064] As described above, the first water separation unit 121 separates the neutralization unit 11 and the second water separation unit 122. Therefore, the kinetic energy of the neutralization mixture 21 flowing into the second water separation unit 122 is reduced, and the neutralization mixture 21 is further and more rapidly and clearly fractionated into the suspension layer 22 and the aqueous layer 23. The first discharge pump 171, connected to the side wall of the second water separation unit 122, then discharges the result from the suspension layer 22 to the outside. The discharged result undergoes the next steps of a purification step to remove alcohol and a filtration step to produce a final product which can be used as a plasticizer. The second discharge pump 172, connected to the bottom surface 14 of the water separation unit 12, then discharges the salt 24 contained in the aqueous layer 23 and precipitated to the outside.

[0065] In the manner described above, both the neutralization reaction and water separation occur smoothly, increasing efficiency. Furthermore, since the neutralization section 11 and the water separation section 12 are integrated into a single neutralization / water separation tank 1, a separate transfer pump is not required, thus preventing an increase in total volume, simplifying the structure, and preventing the accumulation of salt 24.

[0066] Figure 4 is a schematic diagram of a neutralization / water separation tank 1a according to a second embodiment of the present invention.

[0067] According to the first embodiment of the present invention, a circulation pump 16 is connected to the neutralization unit 11. Such a circulation pump 16 discharges the neutralization mixture 21 from the neutralization unit 11 and puts the neutralization mixture 21 back into the neutralization unit 11. As a result, the neutralization mixture 21 can be quickly and uniformly stirred and neutralized.

[0068] However, in the neutralization / water separation tank 1a according to the second embodiment of the present invention, a propeller agitator 18 is connected to the neutralization section 11, as shown in Figure 4. The propeller agitator 18 is an agitator that stirs the liquid by rotating a long rod, which has at least one propeller formed on it, and is installed so that the propeller is immersed in the liquid. Such a propeller agitator 18 may have two propellers, as shown in Figure 4, but is not limited to this, and can have various numbers of propellers. Also, the propeller agitator 18 may be installed approximately vertically in the neutralization section 11, but is not limited to this, and may be installed in various ways, such as at an angle or horizontally.

[0069] By installing such a propeller agitator 18, the total volume of the neutralization / water separation tank 1 can be reduced compared to the circulation pump 16, making installation easier and allowing the neutralization mixture 21 to be stirred more quickly and uniformly.

[0070] According to the first embodiment of the present invention, the first inlet 151 and the second inlet 152 may be connected in between, and the unrefined product mixture, neutralizing agent, and water may be pre-mixed and introduced into the neutralization tank via the third inlet 153. However, according to the second embodiment of the present invention, a propeller agitator 18 is used instead of the circulation pump 16, so that the neutralization mixture 21 can be stirred more quickly and uniformly. Therefore, since it is not necessary for the first inlet 151a and the second inlet 152a to be connected in between, the unrefined product mixture can be introduced into the neutralization tank separately via the first inlet 151a, and the neutralizing agent and water can be introduced separately via the second inlet 152a.

[0071] Figure 5 is a schematic diagram of the neutralization / water separation tank 1b according to the third embodiment of the present invention.

[0072] According to the first and second embodiments of the present invention, the bottom surfaces 14 of the neutralization / water separation tanks 1 and 1a are formed flat. However, if the bottom surface 14 of the water separation section 12 is flat, the precipitated salt 24 will be dispersed on the bottom surface 14 of the water separation section 12. Therefore, it may not be easy for the second discharge pump 172 to discharge the salt 24 to the outside.

[0073] In the third embodiment of the present invention, the neutralization / water separation tank 1b may be formed such that the bottom surface 141 of the water separation section 12a slopes downward toward the center, as shown in Figure 5. That is, the bottom surface 141 of the water separation section 12a may have a conical shape. The second discharge pump 172 may be connected to the center of the bottom surface 141 of the water separation section 12a. As a result, when the salt 24 settles, it will collect at the center of the bottom surface 141 of the water separation section 12a, and the second discharge pump 172 can easily discharge the settled salt 24 to the outside.

[0074] On the other hand, if the neutralization / water separation tank 1 stops operating, salt 24 may also precipitate in the neutralization section 11. However, according to the first and second embodiments of the present invention, since the bottom surface 14 of the neutralization section 11 is flat, the precipitated salt 24 is dispersed on the bottom surface 14 of the neutralization section 11. In particular, if the neutralization / water separation tank 1 stops operating for a long period of time, the precipitated salt 24 may accumulate and solidify in the corners of the bottom surface 14 of the neutralization section 11. In that case, even if the neutralization / water separation tank 1 starts operating again, the salt 24 may not be mixed into the neutralization mixture 21 and may remain in the corners of the bottom surface 14 of the neutralization tank.

[0075] In the third embodiment of the present invention, the neutralization / water separator tank 1b, as shown in Figure 5, may also be formed such that the bottom surface 142 of the neutralization section 11a is inclined downwards toward the center. That is, the bottom surface 142 of the neutralization section 11a may also have a conical shape. The circulation pump 16 may be connected to the center of the bottom surface 142 of the neutralization section 11a. As a result, even if the neutralization / water separator tank 1 is stopped from operating for a long period of time, the precipitated salt 24 will collect at the center of the bottom surface 142 of the neutralization section 11a. When the neutralization / water separator tank 1 is started again, the circulation pump 16 will discharge the neutralization mixture 21 along with the precipitated salt 24 from the neutralization section 11a, and the neutralization mixture 21 can be put back into the neutralization section 11a. Therefore, it is possible to prevent the precipitated salt 24 from accumulating and solidifying on the bottom surface 142 of the neutralization section 11a.

[0076] Figure 6 is a schematic diagram of a neutralization / water separation tank 1c according to the fourth embodiment of the present invention.

[0077] In the fourth embodiment of the present invention, the neutralization / water separation tank 1c, as shown in Figure 6, has a propeller agitator 18 connected to the neutralization section 11a. This allows for a reduction in the total volume of the neutralization / water separation tank 1 compared to the circulation pump 16, making installation easier and enabling more rapid and uniform stirring of the neutralization mixture 21.

[0078] Furthermore, the bottom surface 141 of the water separation section 12a may be formed to slope downwards towards the center. The second discharge pump 172 may be connected to the center of the bottom surface 141 of the water separation section 12a. As a result, when the salt 24 settles, it will collect at the center of the bottom surface 141 of the water separation section 12a, and the second discharge pump 172 will be able to easily discharge the settled salt 24 to the outside.

[0079] Furthermore, the bottom surface 142 of the neutralization section 11a may be formed to slope downwards towards the center. The circulation pump 16 may be connected to the center of the bottom surface 142 of the neutralization section 11a. This prevents the salt 24 precipitated on the bottom surface 142 of the neutralization section 11a from accumulating and solidifying.

[0080] A person with ordinary skill in the art to which the present invention pertains will understand that the present invention may be carried out in other specific forms without altering its technical idea or essential features. Therefore, the embodiments described above should be understood to be illustrative and not restrictive in all respects. The scope of the present invention is indicated more by the claims described below than by the detailed description above, and the meaning and scope of the claims, and the various embodiments derived from the concept of equivalents thereto, should be interpreted as being included within the scope of the present invention.

Claims

1. A neutralization unit into which an unrefined product mixture containing an alcohol and an ester compound, a neutralizing agent, and water are added to form a neutralized mixture, A water separation unit that separates the neutralized mixture into a floating layer and a water layer, A first partition wall extends upward from the bottom surface to form an upper passage, separating the neutralization section and the water separation section, It includes a second partition wall that extends downward from the ceiling and forms a lower passage, The water separation unit is The neutralization mixture flows from the neutralization section through the upper passage to the first water separation section, The neutralization mixture is introduced into a second water separation section from the first water separation section via the lower passage, and the following are included: The first water separation unit and the second water separation unit are Separated by the second partition, The water separation unit further includes a second discharge pump that discharges the salt contained in the aqueous layer and settled to the outside from the bottom surface of the water separation unit, The bottom surface of the water separation section is It is formed with a downward slope as it approaches the center. The bottom surface of the neutralization section is It is formed with a downward slope as it approaches the center. The second discharge pump is connected to the center of the bottom surface of the water separation section. Neutralization / water separation tank for esterification products.

2. The neutralization / water separation tank for esterification products according to claim 1, further comprising a first discharge pump for discharging the resulting product contained in the suspended layer to the outside from the side wall of the second water separation section.

3. The neutralization / water separation tank for esterification products according to claim 1, further comprising a circulation pump for discharging the neutralized mixture from the neutralization section and returning the neutralized mixture to the neutralization section.

4. The neutralization / water separation tank for esterification products according to claim 1, further comprising a propeller agitator installed in the neutralization section for stirring the neutralized mixture.

5. The aforementioned slope is, A neutralization / water separation tank for esterification products according to claim 1, wherein the temperature is 5 to 45°.

6. The aforementioned upper passageway is The neutralization / water separation tank for esterification products according to claim 1, having a height of 10 to 50% of the height of the first partition wall.

7. The aforementioned lower passageway is The neutralization / water separation tank for esterification products according to claim 1, having a height of 10 to 50% of the height of the second partition wall.

8. The process involves adding an unrefined product mixture containing alcohol and an ester compound, a neutralizing agent, and water to the neutralization section of a neutralization / water separation tank. The steps include mixing the unpurified product mixture, the neutralizing agent, and the water to form a neutralized mixture, The neutralization mixture flows into the first water separation section of the water separation section via the upper passage, The neutralization mixture flows into the second water separation section of the water separation section via the lower passage, The steps include: separating the neutralized mixture into a floating layer and an aqueous layer; The steps include: discharging the resulting material contained in the floating layer to the outside; The steps include: discharging the salt contained in the aqueous layer and precipitated to the outside via the second discharge pump; including, A method for neutralizing and separating esterification products using a neutralization / water separation tank for esterification products according to any one of claims 1 to 7.

9. In the step of forming the neutralized mixture, The method for neutralizing and separating water from an esterification product according to claim 8, wherein a circulation pump discharges the neutralized mixture from the neutralization section and then puts the neutralized mixture back into the neutralization section.

10. In the step of forming the neutralized mixture, The method for neutralizing and separating an esterification product from water according to claim 8, wherein the neutralization mixture is stirred using a propeller agitator.

11. The salts that precipitated in the aqueous layer are The method for neutralizing and separating esterification products according to claim 8, wherein the product is collected at the center of the bottom surface of the water separation section.

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