Refinery apparatus

WO2025063453A1PCT designated stage expired Publication Date: 2025-03-27LG CHEM LTD
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Patent Information

Application Number
PCT/KR2024/009905
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-07-09
Filing Date
2024-07-11
Publication Date
2025-03-27

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Abstract

The present invention relates to a refining apparatus including a distillation column in which the lower area of the column is partitioned into a first area and a second area while having a separation wall interposed therebetween. The distillation column includes: a feed supply port provided in one side part of an intermediate area thereof to supply, to the distillation column, a feed stream containing a material to be refined; a first discharge port provided below the first area; a second discharge port provided below the second area and connected to one side of a reboiler; and a reflux inlet port provided above the second area and connected to the other side of the reboiler, wherein multiple trays arranged to be spaced apart from each other in the vertical direction of the separation wall are provided in the intermediate area of the distillation column; one terminal end of the lowest tray among the multiple trays is open so as not to come into contact with the side part on the first area of the distillation tower; and a guide partition wall is provided to extend downward from the one terminal end of the lowermost tray so as to be adjacent to the bottom of the distillation column.
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Description

refinery

[0001] Cross-citation with related applications

[0002] This application claims the benefit of priority to Korean Patent Application No. 10-2023-0124688, filed September 19, 2023, and Korean Patent Application No. 10-2024-0090008, filed July 9, 2024, the entire contents of which are incorporated herein by reference.

[0003] Technology field

[0004] The present invention relates to a purification device, and more particularly, to a purification device capable of removing inorganic impurities from a feed stream containing inorganic impurities.

[0005] Typically, compounds are produced by mixing multiple substances and conducting multiple reactions. These multiple reaction processes generate unnecessary substances, which reduces product production efficiency. In particular, when producing compounds through reactions involving catalysts, the inclusion of inorganic impurities reduces the purity of the product. Therefore, to obtain high-purity products, it is necessary to remove these unnecessary impurities.

[0006] For example, when producing isopropyl alcohol (IPA), referring to FIG. 1, typically, a propylene monomer and water are reacted in a reaction unit (1) to obtain a reaction product including isopropyl alcohol, unreacted propylene monomer, unreacted water, n-propyl alcohol (NPA), and by-products such as organic substances, and the reaction product is transferred to a gas purification unit (2) to separate low-boiling-point gas components including unreacted propylene monomer, and then the reaction product from which the gas components have been separated is supplied to an IPA purification unit (3) including a plurality of distillation columns to remove organic substances, NPA, and water, thereby obtaining crude isopropyl alcohol. Here, the crude isopropyl alcohol obtained through the gas purification unit and the IPA purification unit may still contain trace amounts of organic substances and water, and in particular, there is a problem of including inorganic impurities such as metal components due to the catalyst used in the reaction.

[0007] The problem to be solved in the present invention is to provide a purification device capable of obtaining a purified substance with high purity by effectively removing inorganic substances remaining in a feed stream containing a purified substance using a purification device having an improved structure of the bottom region of a distillation column in order to solve the problem mentioned in the background technology of the above invention.

[0008] However, the problems that the present invention seeks to solve are not limited to the problems mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the description below.

[0009] According to one embodiment of the present invention for solving the above problem, the present invention provides a purification apparatus including a distillation column and a reboiler, wherein the interior of the distillation column is divided into a bottom region, a middle region, and a top region, and the bottom region may include a first region and a second region separated by a dividing wall extending from the bottom of the distillation column to have a predetermined height therein.

[0010] In addition, the distillation column may include a feed supply port provided at one side of the middle region and supplying a feed stream containing a material to be purified to the distillation column; a first discharge port provided at a lower portion of the first region; a second discharge port provided at a lower portion of the second region and connected to one side of the reboiler; and a reflux inlet provided at an upper portion of the second region and connected to the other side of the reboiler.

[0011] In addition, the purification device according to the present invention is characterized in that a plurality of trays are provided in the middle region of the distillation column and are spaced apart in the vertical direction of the dividing wall, and one end of the lowest tray among the plurality of trays is opened so as not to come into contact with the side of the distillation column on the first region, and a guide baffle is provided extending downward from one end of the lowest tray to be adjacent to the bottom of the distillation column.

[0012] According to the present invention, by using a purification device that improves the structure of the bottom region of a distillation column, inorganic substances remaining in the substance to be purified can be effectively removed, thereby purifying the substance to a high purity.

[0013] More specifically, the purification device according to the present invention can minimize the content of inorganic substances flowing into the reboiler by separating the feed inlet zone and the reboiler zone in the sump by providing a separating wall in the bottom region of the distillation column.

[0014] Furthermore, the purification device according to the present invention can maximize the inorganic material removal rate by precipitating high-density inorganic materials in the material to be purified downwards and then discharging them downwards by means of a guide baffle provided on the lowermost tray and extended adjacent to the bottom of the distillation column.

[0015] The effects that can be obtained from this invention are not limited to the effects mentioned above, and other effects not mentioned can be clearly understood by those skilled in the art to which the present invention pertains from the description below.

[0016] Figure 1 illustrates a typical process for producing crude isopropyl alcohol as an example of a material to be purified.

[0017] Figure 2 is a structural diagram schematically illustrating the overall structure of a purification device according to one embodiment of the present invention.

[0018] Figure 3 is a structural diagram centered on the bottom region of a distillation column among purification devices according to one embodiment of the present invention.

[0019] Figure 4 is a structural diagram centered on the bottom region of a distillation column among purification devices according to one embodiment of the present invention.

[0020] Figure 5 is a structural diagram centered on the bottom region of a distillation column among purification devices according to a comparative example.

[0021] The terms or words used in the description and claims of the present invention should not be interpreted as limited to their usual or dictionary meanings, but should be interpreted as meanings and concepts that conform to the technical idea of ​​the present invention, based on the principle that the inventor can appropriately define the concept of the term to explain his or her own invention in the best way.

[0022] In connection with the description of the drawings, similar reference numerals may be used for similar or related components.

[0023] The singular form of a noun corresponding to an item may include one or more of said items, unless the relevant context clearly indicates otherwise.

[0024] In this disclosure, each of the phrases "A or B", "at least one of A and B", "at least one of A or B", "A, B, or C", "at least one of A, B, and C", and "at least one of A, B, or C" may include any one of the items listed together in the corresponding phrase, or all possible combinations thereof.

[0025] The term “and / or” includes any combination of a plurality of related described elements or any one of a plurality of related described elements.

[0026] Terms such as "first," "second," or "first" or "second" may be used simply to distinguish one component from another and do not qualify the components in any other respect (e.g., importance or order).

[0027] In addition, terms such as 'front', 'rear', 'top', 'bottom', 'side', 'left', 'right', 'upper', and 'lower' used in this application are defined based on the drawings, and the shape and position of each component are not limited by these terms.

[0028] The terms “include” or “have” are intended to specify the presence of a feature, number, step, operation, component, part or combination thereof described in the present disclosure, but do not preclude the presence or addition of one or more other features, numbers, steps, operations, components, parts or combinations thereof.

[0029] When a component is said to be “connected,” “coupled,” “supported,” or “in contact with” another component, this includes not only cases where the components are directly connected, coupled, supported, or in contact, but also cases where the components are indirectly connected, coupled, supported, or in contact through a third component.

[0030] When we say that a component is “on” another component, this includes not only cases where the component is in contact with the other component, but also cases where there is another component between the two components.

[0031] In addition, the terms "about", "substantially", etc. used herein are used in the sense of or close to the numerical value when manufacturing and material tolerances inherent to the meanings mentioned are presented, and are used to prevent unscrupulous infringers from unfairly using the disclosure contents in which exact or absolute numerical values ​​are mentioned to aid understanding of the present invention.

[0032] The term "stream" as used herein may refer to the flow of fluid within a process, or may refer to the fluid itself flowing within a pipe. Specifically, the stream may refer to both the fluid itself flowing within the pipe connecting each device and the flow of the fluid. Furthermore, the fluid may include one or more components of gas, liquid, and solid.

[0033] Additionally, “pressure” as referred to herein means gauge pressure measured based on atmospheric pressure.

[0034] The material to be purified as referred to herein may include a target product, a low-boiling-point organic substance, a high-boiling-point organic substance, and an inorganic substance, wherein the low-boiling-point organic substance may refer to an organic substance having a relatively low boiling point compared to the product, and the high-boiling-point organic substance may refer to an organic substance having a relatively high boiling point compared to the product.

[0035] The purification device of the present invention will be described below with reference to the attached drawings. However, the attached drawings are exemplary and the scope of the purification device is not limited thereto. Furthermore, while isopropyl alcohol is exemplified as the target product, the target material for purification in the purification device according to the present invention is not limited thereto.

[0036] FIG. 2 is a drawing exemplarily showing a purification device and process flow according to one embodiment of the present invention, and FIGS. 3 and 4 are drawings exemplarily showing a detailed structure of a bottom region (A) of a distillation tower (100) according to one embodiment of the present invention.

[0037] Referring to FIG. 2, a purification device according to one embodiment of the present invention includes a distillation column (100). The distillation column (100) is a device capable of separating multi-component substances contained in a raw material based on their respective boiling point differences. Depending on the boiling points of the components of the incoming raw material or the components to be separated, a distillation column equipped with various types of trays may be utilized in the purification device of the present invention.

[0038] A purification device according to one embodiment of the present invention may be equipped with a reboiler (200) that transfers heat to the bottom discharge stream of the distillation tower (100). The reboiler (200) is a heating device separately installed outside the distillation tower (100), and may refer to a device for reheating and evaporating the flow of a substance to be purified that has flowed out from the bottom of the distillation tower.

[0039] If necessary, the purification device may further be equipped with a condenser (not shown) for converting the upper discharge stream of the distillation column (100) into a liquid phase. The condenser is a device separately installed outside the distillation column (100), and refers to a device for cooling the stream discharged from the top of the distillation column, for example, by contacting it with cooling water introduced from the outside.

[0040] Referring to FIG. 2, the interior of the distillation tower (100) can be divided into a bottom region (A), a middle region (B), and a top region (C).

[0041] In this specification, the term “bottom region” means a relatively lower part in the structure of the distillation column (100), and may mean, for example, the lowest part among three regions divided in the height direction of the distillation column (100), and more specifically, may mean the region below the lowest tray.

[0042] In addition, the term “top region” in this specification means a relatively upper part in the structure of the distillation column (100), and may mean, for example, the uppermost part among three regions divided in the height direction of the distillation column (100), and more specifically, may mean the region above the uppermost tray.

[0043] In addition, in this specification, the “middle region” means a relatively central part in the structure of the distillation column (100), and may mean, for example, a middle region among three regions divided in the height direction of the distillation column (100), and more specifically, may mean a region between the bottom region (A) and the top region (C) of the distillation column (100), i.e., a region between the bottom tray and the top tray.

[0044] In this specification, the bottom region, top region, and middle region of the distillation column may be used as relative concepts. The lower part of the distillation column (100) is included in the bottom region, and the upper part of the distillation column (100) is included in the top region. Unless specifically defined otherwise in this specification, the bottom region (A) is used with the same meaning as the lower region, and the top region (C) is used with the same meaning as the upper region.

[0045] In addition, a dividing wall (110) extending from the bottom of the distillation tower to a sump where a liquid feed is collected is provided inside the bottom region (A) of the distillation tower (100) to have a predetermined height, and the sump region is divided into a first region (D1) and a second region (D2) with the dividing wall (110) interposed therebetween. Here, the sump region may refer to the bottom region (A). In addition, the bottom region (A) may also be divided into a liquid region and a gaseous region based on the liquid surface of the solution.

[0046] The height of the above-described dividing wall (110) can be appropriately changed depending on the structure or size of the distillation column. However, as illustrated in FIG. 2, it can be provided so as not to be in contact with the lowermost tray (120) described later. Here, the predetermined height may mean a height at which the dividing wall (110) is spaced apart from the lowermost tray (120) so as not to be in contact with it. In addition, since the upper end of the dividing wall (110) is provided so as not to be in contact with the lowermost tray (120), the gas in the gas phase region of the bottom region (A) can move between the first region (D1) and the second region (D2).

[0047] Meanwhile, referring to FIG. 3, the first region (D1) and the second region (D2) may be partitioned unequally as needed. More specifically, the volume of the first region (D1) may be determined according to the flow rate of the stream discharged below the second region (D2) and the rate at which inorganic substances precipitate in the first region (D1). In addition, the first region (D1) and the second region (D2) are preferably partitioned so that the solution contained in the first region (D1) overflows into the second region (D2), and the solution in the second region (D2) does not flow into the first region (D1).

[0048] Referring to Figure 5, in the past, there was no separation wall in the distillation tower sump, so the section where the feed, which is the material to be purified, flows into the sump and the bottom discharge stream (reboiler section) that is circulated to the reboiler for gas-liquid separation were not separated from each other, but coexisted in a structure where the bottom discharge stream that is circulated to the reboiler contains inorganic substances and passes through the reboiler. In this way, when the inorganic substances enter the reboiler, they are entrained in the gas phase of the reflux stream of the gas-liquid mixed phase that is generated as they are heated while passing through the reboiler and move upward, which has the problem of lowering the purity of the purified product.

[0049] In order to solve such a problem, the present invention provides a device capable of purifying a substance to be purified with high purity by dividing the sump into a first region (D1), which is a feed inlet region and an inorganic material removal region, and a second region (D2), which is a reboiler region, by providing a dividing wall (110) in the bottom region (A) of the distillation column (100), thereby minimizing the inorganic material content introduced into the bottom discharge stream circulated to the reboiler. In addition, a vertical mixed flow occurs in the solution inside the second region (D2) due to the bottom discharge stream of the second region (D2) and the liquid reflux stream introduced into the second region (D2), but the solution inside the first region (D1) can have a gentle flow without being affected by the flow of the solution inside the second region (D2) due to the dividing wall (110) located between the first region (D1) and the second region (D2), so that inorganic materials with a relatively high density can be precipitated in the lower part of the first region (D1). At this time, the precipitated inorganic matter can be discharged together with high-boiling-point organic matter through the first discharge port (102) described later.

[0050] In a purification device according to one embodiment of the present invention, referring to FIG. 2, a distillation column (100) is provided with a feed supply port (101), and further, first and second discharge ports (102, 103) and a reflux inlet (104) may be provided in a lower region of the distillation column, and a third discharge port (105) may be further provided in an upper region of the distillation column.

[0051] The above feed supply port (101) is provided at one side of the distillation column (100). A feed stream containing a substance to be purified can be supplied to the distillation column (100) through the feed supply port (101). In FIG. 2, the feed supply port (101) is illustrated as being located in the middle region (B) of the distillation column, but is not limited thereto, and its height (number of stages) can be appropriately selected depending on the composition, temperature, and pressure of the feed. For example, the energy consumption of the reboiler varies depending on the composition, temperature, and pressure of the feed, and accordingly, the height of the feed supply port (101) can be determined.

[0052] The above-mentioned purification target material can be purchased as a commercially available material or can be manufactured by a method conventional in the field. At this time, the purification target material may contain inorganic substances as impurities in an amount of more than 0 ppb and less than or equal to 100 ppb. For example, the inorganic substances may include one or more metal components selected from aluminum (Al), arsenic (As), iron (Fe), boron (B), chromium (Cr), cadmium (Cd), titanium (Ti), zinc (Zn), and magnesium (Mg). The type and content of impurities contained in the purification target material may vary depending on various environments accompanying the reaction and purification processes.

[0053] In one embodiment, when the material to be purified is a crude isopropyl alcohol, referring to FIG. 1, a reaction unit (1) reacts a propylene monomer with water to obtain a reaction product including isopropyl alcohol (IPA) along with unreacted propylene monomer, unreacted water, n-propyl alcohol (NPA), and by-products such as organic substances, and then the reaction product is transferred to a gas purification unit (2) including an absorption tower, a gas purification tower, etc., to separate low-boiling-point gas components including unreacted propylene monomer. The reaction product (including IPA, NPA, water, and organic substances) from which the gas components have been separated is supplied to an IPA purification unit (3), and the crude isopropyl alcohol can be obtained by removing organic substances, NPA, and water through a purification process performed in a plurality of distillation columns.

[0054] The above isopropyl alcohol crude product may be obtained by supplying the reaction product of propylene and water to a gas purification unit and an IPA purification unit to separate gas components, organic substances, etc., but may still contain trace amounts of organic substances and water, and in particular, may contain inorganic impurities including metal components such as Al, As, Fe, B, Cr, Cd, Ti, Zn, and Mg due to the use of a catalyst during the reaction.

[0055] For example, the crude isopropyl alcohol product may contain, as impurities, 0.08 wt% or less of low-boiling-point organic substances, 0.05 wt% or less of high-boiling-point organic substances, and 100 ppb or less of inorganic substances, based on the total weight thereof. The low-boiling-point organic substances may include, for example, an inert gas having C3 or less, and acetone, and the high-boiling-point organic substances may include, for example, n-propyl alcohol, and hexanol, and the inorganic substances may include, for example, metal components such as Al, As, Fe, B, Cr, Cd, Ti, Zn, and Mg, but are not limited thereto.

[0056] To remove inorganic substances contained in a material to be purified, the present invention provides a purification device capable of recovering a highly purified product by improving the structure of the bottom region (A) of the distillation column. The distillation column usable in the present invention may have a structure that is identical to that commonly used in petrochemical processes, except for the structure of the bottom region, without any particular limitations.

[0057] Meanwhile, a plurality of trays in the form of a perforated plate or grid are provided in the middle region (B) of the distillation column (100), and a plurality of stages are defined by the plurality of trays. The plurality of trays are arranged in a vertical direction with respect to the height direction of the distillation column and are spaced apart from each other. In each stage, a gaseous stream rising upward and a liquid stream descending downward come into contact with each other to transfer heat and mass, and as a result, a part of a high-boiling-point component is condensed and flows down to the bottom, and a process in which the uncondensed vapor continues to rise to the top is continuously performed.

[0058] The number, type, and size of the plurality of trays are not particularly limited, and can be set based on the number of theoretical plates inferred from a distillation curve considering the composition of the feed stream. As used herein, the term “number of theoretical plates” refers to a virtual area in which two phases, such as a gas phase and a liquid phase, are in equilibrium with each other in a distillation column (100) or the number of stages partitioned by a plurality of trays. For example, a distillation column having 40 to 60 theoretical plates can be used as the distillation column (100).

[0059] Meanwhile, in a purification device according to one embodiment of the present invention, one end of the lowest tray (120), which is a collector tray among the plurality of trays, is positioned above the first region (D1), and a guide partition (130) is provided extending downward from the one end of the lowest tray (120) to be adjacent to the bottom of the distillation column. One end of the lowest tray (120) is open so as not to come into contact with the side of the distillation column (100) on the first region (D1). Here, a descending liquid stream among the feed streams containing the material to be purified can be introduced into the first region (D1) through the guide partition (130).

[0060] In addition, the lower end of the guide partition wall (130) is located below the upper end of the separation wall (110), i.e., the liquid level of the solution in the first region (D1). In addition, as shown in FIGS. 3 and 4, the first region (D1) can be divided into a first-first region (D1-1) and a second-second region (D1-2) by the guide partition wall (130).

[0061] Referring to FIG. 5, in the past, the lower end of the guide baffle was positioned above the liquid surface of the solution in the sump, so that the inorganic substances were maintained in a mixed state in the dropped solution, and the flow of the solution in the sump was active, so that the inorganic substances could not be precipitated. On the other hand, in the present invention, the lower end of the guide baffle (130) was positioned below the liquid surface of the solution in the first region (D1), so that the precipitation of inorganic substances having a relatively high density could be induced, and the 1-1 region (D1-1), into which the descending liquid stream among the feed streams flows, and the 1-2 region (D1-2), where the inorganic substances in the solution are precipitated, could be separated.

[0062] Specifically, after the descending liquid stream among the feed streams flows into the 1-1 region (D1-1), a flow is generated that moves to the 1-2 region (D1-2) through the space separated between the bottom of the distillation column and the guide partition. At this time, the solution in the 1-2 region (D1-2) can maintain a smooth flow because the influence of the solution flow that drops into the 1-1 region (D1-1) by the guide partition (130) is minimized, and accordingly, precipitation of relatively dense inorganic substances can occur in the 1-2 region (D1-2). Furthermore, the precipitated inorganic substances are discharged as a lower discharge stream of the 1st region, and when the liquid stream flows in such a way as to exceed the internal capacity of the 1st region (D1), the solution in the upper part of the 1-2 region (D1-2) where the inorganic substances are minimized flows over to the 2nd region (D2). Accordingly, the inorganic matter in the lower discharge stream of the second region circulated to the reboiler (200) is minimized, and the inorganic droplet entrainment in the reflux stream of the gas passing through the reboiler is minimized, thereby further improving the purity of the purified product.

[0063] More specifically, the height (h) from the bottom of the distillation column to the lower end of the guide bulkhead can satisfy the following equation (1).

[0064] Equation (1): 0.5d < h < 2d

[0065] Here, d is the maximum open gap between one end of the lowermost tray and the side of the distillation column.

[0066] When the height (h) from the bottom of the distillation column to the lower end of the guide baffle satisfies the range of the above equation (1), the influence of the solution flow in the 1-2 region (D1-2) by the flow moving from the 1-1 region (D1-1) to the 1-2 region (D1-2) can be minimized. That is, the flow moving from the 1-1 region (D1-1) to the 1-2 region (D1-2) can be maintained in a calm state, thereby suppressing the mixing flow of the solution in the 1-2 region (D1-2) and inducing the precipitation of inorganic substances.

[0067] Meanwhile, referring to FIG. 4, a magnetic bar (111) for removing inorganic substances may be further provided on at least one side of the separation wall (110). When the magnetic bar (111) is provided, the removal efficiency of inorganic substances having magnetism, such as iron (Fe) and magnetite, contained in the solution can be improved. As described above, since inorganic substances having a relatively high density are precipitated in the first region (D1), it may be preferable for the magnetic bar (111) to be located in the first region (D1) in terms of inorganic substance removal efficiency, but the present invention is not limited thereto. For example, when the magnetic bar (111) is located in the first region (D1), inorganic substances having magnetism may be attached to the magnetic bar or guided to the lower part of the first-second region (D1-2), thereby facilitating discharge through the first discharge port (102) described later.

[0068] The first discharge port (102) is located at the bottom of the first region (D1) and can discharge the lower discharge stream of the first region (D1) containing the high-boiling-point organic matter and inorganic matter. A descending liquid stream among the feed stream containing the material to be purified flows into the first region (D1) through the guide partition wall (130), and the solution flowing into the first region (D1) contains high-boiling-point organic matter and inorganic matter. A portion of the solution flowing into the first region (D1) is discharged through the first discharge port (102) as the lower discharge stream of the first region (D1), and the remaining solution exceeding the internal capacity of the first region (D1) flows into the second region (D2). Here, a gentle solution flow is formed within the first-second region (D1-2), so that the inorganic matter precipitates downward, and thus, most of the inorganic matter can be included in the lower discharge stream of the first region (D1) and discharged. More specifically, since more inorganic substances are deposited, especially in the lower part of the first-second region (D1-2), by the guide partition (130), the efficiency of removing inorganic substances can be further improved when the first discharge port (102) is located in the lower part of the first-second region (D1-2).

[0069] For example, the high boiling point organic matter discharged through the first discharge port (102) may include n-propyl alcohol, hexanol, or a mixture thereof, and the inorganic matter may include one or more metal components selected from Al, As, Fe, B, Cr, Cd, Ti, Zn, and Mg.

[0070] Meanwhile, as illustrated in FIG. 4, the flow rate of the lower discharge stream of the first region (D1) can be controlled using a level control valve, and specifically, the flow rate of the lower discharge stream of the first region (D1) discharged through the first discharge port (102) can be controlled according to the water level of the solution in the second region (D2).

[0071] The second outlet (103) is provided at the lower portion of the second region (D2) and is connected to one side of the reboiler (200). The solution of the first region (D1) flows into the second region (D2) over the separation wall (110), and the solution in the second region (D2) is discharged through the second outlet (103), passes through the reboiler (200), and is then recycled through the reflux inlet (104) described later and flows back into the second region (D2). At this time, the solution flowing from the first region (D1) to the second region (D2) may be in a state where most of the inorganic substances have been removed.

[0072] The reflux inlet (104) is located at the upper portion of the second region (D2) and is connected to the other side of the reboiler (200). More specifically, the reflux inlet (104) may be located at a height between the lowermost tray (120) and the liquid surface of the solution in the second region (D2). The gas-liquid mixed phase stream that has passed through the reboiler (200) through the reflux inlet (104) may be refluxed to the bottom region (A) of the distillation column. The liquid in the refluxed gas-liquid mixed phase stream moves downward and is received in the second region (D2), and the vapor moves to the upper middle region (B) and undergoes a gas-liquid separation process.

[0073] The reflux inlet (104) may further be provided with a pipe (104a) extending inwardly of the distillation column. The extension pipe (104a) may be provided in a horizontal direction. The flow of the liquid phase moving downward among the refluxed gas-liquid mixed phase stream through the extension pipe (104a) is induced to descend adjacent to the inclined baffle (140) described later, thereby preventing the flow of the liquid phase among the refluxed gas-liquid mixed phase stream from being mixed by crossing over to the first region (D1), and at the same time, the flow of the liquid phase among the refluxed gas-liquid mixed phase stream can be induced to gently flow to the second region (D2).

[0074] As illustrated in FIG. 4, if necessary, a slope baffle (140) may be further provided within the bottom region (A) of the distillation column (100). The reflux stream introduced through the reflux inlet (104) has a large flow rate and a high flow rate, so that some of the reflux stream may flow over to the first region (D1) and affect the flow of the solution within the first region (D1), which may hinder the smooth flow of the solution within the first region (D1) and prevent the precipitation of inorganic substances. In addition, the reflux stream may be mixed with the solution introduced from the lowermost tray (i.e., collector tray) (120) and the inorganic substances may be introduced into the second region (D2). At this time, if the slope baffle (140) is provided, the reflux stream may be prevented from being mixed with the solution introduced from the lowermost tray (120) or the solution within the first region (D1). In addition, the descending liquid phase flow among the refluxed gas-liquid mixed phase stream can be induced to flow gently to the second region (D2) by passing through the inclined baffle (140).

[0075] In detail, the inclined baffle (140) may be provided so as to be positioned at a height between the reflux inlet (104) and the upper end of the separation wall (110). More specifically, one end of the inclined baffle (140) may be positioned above the first region (D1), and the other end of the inclined baffle (140) may be positioned above the second region (D2). In addition, it is preferable that the other end of the inclined baffle located above the second region (D2) be positioned at a lower height than the one end of the inclined baffle located above the first region (D1) so that the solution coming into contact with the inclined baffle (140) can be guided to the second region (D2). For example, the inclination of the inclined baffle (140) may be 5° to 30°, specifically, 10° to 25°, and more specifically, 15° to 20°. Here, the inclination means the angle of inclination with respect to the horizontal floor.

[0076] In one embodiment, a third outlet (105) may be positioned in the top region (C) of the distillation column. For example, when the material to be purified is an isopropyl alcohol crude product, isopropyl alcohol (IPA) and / or low-boiling-point organic substances contained in the isopropyl alcohol crude product may be discharged through the third outlet (105). The low-boiling-point organic substances may include an inert gas having a C3 or lower content, acetone, or a mixture thereof.

[0077] In addition, the stream discharged through the third discharge port (105) passes through a condenser (not shown), some of which is discharged, and the remainder is converted into a liquid phase and can be refluxed back to the distillation tower (100) through the inlet port (106) provided in the top region (C).

[0078] For example, the material to be purified supplied to the distillation column (100) undergoes a separation process through continuous gas-liquid contact in each stage included in the intermediate region (B), and relatively low-boiling-point organic substances and products (e.g., isopropyl alcohol) rise in a vapor state and are discharged through the third outlet (105) of the top region (C), and relatively heavy components, high-boiling-point organic substances and inorganic substances, descend in a condensed state and are discharged through the first outlet (102) of the bottom region (A). In addition, the effluent of the top region (C) may contain a trace amount of water that was included in the material to be purified. Furthermore, the effluent of the top region (C) may undergo an additional purification process as needed, through which a high-purity product can ultimately be obtained.

[0079] Above, the purification device according to the present invention has been described and illustrated in the drawings, but the description and illustration in the drawings describe and illustrate only the core components for understanding the present invention, and in addition to the processes and devices described and illustrated in the drawings, processes and devices not described and illustrated separately can be appropriately applied and utilized to implement the purification device according to the present invention.

[0080] Although exemplary embodiments of the present invention have been described above, the present invention is not limited thereto, and those skilled in the art will understand that various changes and modifications are possible within the scope and spirit of the claims set forth below.

[0081] [Explanation of symbols]

[0082] 100: Distillation column, 200: Reboiler

[0083] A: bottom area, B: middle area, C: top area

[0084] D1: Area 1, D2: Area 2

[0085] D1-1: Area 1-1, D1-2: Area 1-2

[0086] 101: Feed supply port, 102: First discharge port

[0087] 103: Second outlet, 104: Reflux inlet, 104a: Extension pipe

[0088] 110: Separating wall, 111: Magnetic bar

[0089] 120: Bottom tray, 130 guide bulkhead, 140: Inclined baffle

Claims

1. A purification device including a distillation tower and a reboiler, The interior of the distillation column is divided into a bottom region, a middle region, and a top region, The above-mentioned bottom region includes a first region and a second region separated by a dividing wall extending from the bottom of the distillation column to have a predetermined height therebetween, The above distillation tower, A feed supply port provided on one side of the above intermediate region for supplying a feed stream containing a substance to be purified to the distillation tower; A first discharge port provided at the lower portion of the first region; A second discharge port provided at the lower portion of the second region and connected to one side of the regenerator; and A reflux inlet provided on the upper part of the second region and connected to the other side of the regenerator; A purification device, wherein a plurality of trays are provided in the middle region of the distillation column and are spaced apart in the vertical direction of the dividing wall, and one end of the lowest tray among the plurality of trays is open so as not to come into contact with the side of the distillation column on the first region, and a guide baffle is provided extending downward from one end of the lowest tray to be adjacent to the bottom of the distillation column.

2. In paragraph 1, The height (h) from the bottom of the distillation column to the lower end of the guide bulkhead satisfies the following equation (1): Equation (1): 0.5d < h < 2d Here, d is the maximum open gap between one end of the lowermost tray and the side of the distillation column.

3. In paragraph 1, A purification device, wherein the above-mentioned purified material contains inorganic substances as impurities in an amount of more than 0 ppb and less than or equal to 100 ppb based on the total weight thereof.

4. In paragraph 3, A refining device, wherein the above inorganic material comprises one or more metal components selected from Al, As, Fe, B, Cr, Cd, Ti, Zn and Mg.

5. In paragraph 3, A feed stream containing the material to be purified is introduced into the first region through the guide bulkhead, A purification device comprising a lower discharge stream of the first region containing the inorganic material being discharged through the first discharge port.

6. In paragraph 1, A purification device, wherein the reflux inlet further includes a pipe extending inwardly of the distillation column.

7. In paragraph 1, A purification device further comprising an inclined baffle provided at a height between the reflux inlet and the upper end of the separation wall.

8. In paragraph 7, One end of the above inclined baffle is located above the first region, A purification device, wherein the other end of the inclined baffle is located above the second region.

9. In paragraph 7, A purification device in which the inclined baffle is provided so that the other end of the upper portion of the second region is positioned at a lower height than the other end of the upper portion of the first region.

10. In paragraph 1, A purification device further comprising a magnetic bar provided on at least one side of the above separation wall.

11. In paragraph 10, A purification device, wherein the magnetic bar is located in the first region.

Citation Information

Patent Citations

  • Refinery apparatus

    KR1020250042059A

  • Tower cauldron of acetic acid rectifying column

    CN206809811U

  • Method for purifying (meth)acrylic acid esters using a divided-wall column

    JP2022516377A

  • Preparation method for isopropyl alcohol

    KR1020140003337A

  • Method of purification for polymerization solvent of preparing process for petroleum resin using dividing wall column

    KR102414715B1