Purification apparatus

Abstract

The present invention relates to a purification apparatus with an improved structure to effectively remove inorganic substances remaining in a material being purified and, more specifically, to a purification apparatus comprising: inside a lower column region of a distillation column, a first region and a second region partitioned by a dividing wall extending from the bottom of the distillation column to a predetermined height; a first guide partition wall extending downward from one end of a lowermost tray so as to be adjacent to the bottom of the distillation column; a reflux pipe extending from a reflux inlet toward the inside of the distillation column; an inclined baffle positioned at a height between the reflux pipe and the upper end of the dividing wall; and a second guide partition wall spaced apart between the dividing wall and the first guide partition wall and extending downward from one end of the inclined baffle so as to be adjacent to the bottom of the distillation column.

Description

refinery

[0001] Cross-citation with related applications

[0002] This application claims the benefit of priority from Korean Patent Application No. 10-2024-0100001, filed July 29, 2024, the entire contents of which are incorporated herein by reference.

[0003] Technology field

[0004] The present application relates to a purification device, and more specifically, to a purification device capable of effectively removing inorganic impurities from a purification target material containing inorganic impurities.

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

[0006] For example, in a process of producing a desired product by reacting a monomer and water in a reaction unit, a reaction product containing unreacted monomer, unreacted water, byproducts, organic substances, etc. is obtained along with the product. The reaction product is transferred to a gas purification unit to separate low-boiling-point gas components including unreacted monomers. Subsequently, the reaction product from which the gas components have been separated is supplied to a product purification unit including a plurality of distillation columns to remove organic substances and water, thereby obtaining a product. Here, the product obtained through the gas purification unit and the product purification unit may still contain trace amounts of organic substances and water, and in particular, there is a problem of containing inorganic impurities such as metal components due to the catalyst used in the reaction.

[0007] The problem to be solved in the present disclosure is to provide a purification device with an improved structure to effectively remove inorganic substances remaining in a material to be purified, in order to solve the problem mentioned in the background technology of the above invention.

[0008] However, the problems to be solved by the present disclosure 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 disclosure for solving the above problem, a purification device including a distillation column and a reboiler is provided, wherein the interior of the distillation column is divided into a bottom region; a middle region; and a top region, and the middle region of the distillation column includes a feed supply port provided at one side of the middle region for supplying a feed stream containing a substance to be purified to the distillation column; and a plurality of trays spaced apart from each other in the middle region.

[0010] In addition, the bottom region of the distillation column may include a first region and a second region, which are partitioned by a dividing wall extending from the bottom of the distillation column to have a predetermined height therein; a first guide baffle disposed spaced apart from the dividing wall in the first region and extending downward from one end of the lowest tray to be adjacent to the bottom of 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; a reflux inlet provided at an upper portion of the second region and connected to the other side of the reboiler; a reflux pipe extending inward from the reflux inlet in the distillation column; an inclined baffle positioned at a height between the reflux pipe and an upper end of the dividing wall; and a second guide baffle disposed spaced apart from the dividing wall and the first guide baffle and extending downward from one end of the inclined baffle to be adjacent to the bottom of the distillation column.

[0011] In addition, the inclined baffle may include one end positioned above the first region, the other end positioned above the second region, and the other end positioned relatively higher than the one end.

[0012] According to the present disclosure, a purification device having an improved structure in the bottom region of a distillation column can be used to effectively remove inorganic substances remaining in a substance to be purified, thereby enabling purification to be performed at a high purity.

[0013] More specifically, the purification device according to the present disclosure can minimize the content of inorganic substances introduced into the reboiler by separating the feed stream inlet zone (first zone) and the reboiler zone (second zone) within the sump by providing a separation wall in the bottom region of the distillation column. In addition, the first guide baffle extending adjacent to the bottom of the distillation column can cause dense inorganic substances in the material to be purified to precipitate downward and then discharge downward, thereby maximizing the inorganic substance removal rate.

[0014] Furthermore, by providing an inclined baffle and a second guide baffle in the bottom region of the distillation column, the entire amount of the reflux stream of the liquid phase that has passed through the reboiler can be refluxed to the first region, thereby preventing the accumulation of inorganic substances in the second region and the reboiler.

[0015] The effects that can be obtained from the present disclosure are not limited to the effects mentioned above, and other effects that are not mentioned can be clearly understood by a person having ordinary skill in the art to which the present disclosure belongs from the description below.

[0016] FIG. 1 is a structural diagram schematically illustrating the overall structure of a purification device according to one embodiment of the present disclosure.

[0017] Figure 2 is a structural diagram centered on the bottom region of a distillation column among purification devices according to one embodiment of the present disclosure.

[0018] FIG. 3a is a cross-sectional view exemplarily showing a cross-section of a bottom region of a distillation column in one embodiment of the present disclosure.

[0019] FIG. 3b is a cross-sectional view exemplarily showing a cross-section of a bottom region of a distillation column in one embodiment of the present disclosure.

[0020] FIG. 4a is an exemplary diagram illustrating an embodiment of a purification device having a magnetic filter provided in front of a feed supply port according to one embodiment of the present disclosure.

[0021] FIG. 4b is an exemplary diagram illustrating an embodiment of a purification device having a magnetic filter at a rear end of a first discharge port according to one embodiment of the present disclosure.

[0022] FIG. 5 is an exemplary diagram illustrating an embodiment of the present disclosure in which a pipe before a feed supply port or after a first discharge port is branched and a magnetic filter is provided in each pipe.

[0023] FIG. 6 is an exemplary diagram illustrating one aspect of a second guide bulkhead in a purification device according to one embodiment of the present disclosure.

[0024] The terms or words used in the description and claims of this disclosure 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 ​​this disclosure, 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.

[0025] In connection with the description of the drawings, similar reference numerals may be used for similar or related components.

[0026] 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.

[0027] 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.

[0028] The term “and / or” includes any combination of a plurality of related described elements or any one of a plurality of related described elements.

[0029] 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).

[0030] In addition, terms such as 'front', 'rear', 'top', 'bottom', 'side', 'left', 'right', 'upper', and 'lower' used in the present disclosure are defined based on the drawings, and the shape and position of each component are not limited by these terms.

[0031] 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.

[0032] 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.

[0033] 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.

[0034] In addition, the terms "about", "substantially", etc. used in this disclosure 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 this disclosure.

[0035] The term "stream" as used herein may refer to the flow of fluid within a process, and may also 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.

[0036] Additionally, “pressure” as referred to in the present disclosure means gauge pressure measured based on atmospheric pressure.

[0037] The material to be purified as referred to in the present disclosure may include a target product (organic matter), a low-boiling-point organic matter, a high-boiling-point organic matter, and an inorganic matter, wherein the low-boiling-point organic matter may refer to an organic matter having a relatively low boiling point compared to the product, and the high-boiling-point organic matter may refer to an organic matter having a relatively high boiling point compared to the product.

[0038] According to one embodiment of the present disclosure, 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 middle region of the distillation column includes a feed supply port provided at one side of the middle region for supplying a feed stream containing a substance to be purified to the distillation column; and a plurality of trays spaced apart from each other in the middle region.

[0039] In addition, the bottom region of the distillation column may include a first region and a second region, which are partitioned by a dividing wall extending from the bottom of the distillation column to have a predetermined height therein; a first guide baffle disposed spaced apart from the dividing wall in the first region and extending downward from one end of the lowest tray to be adjacent to the bottom of 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; a reflux inlet provided at an upper portion of the second region and connected to the other side of the reboiler; a reflux pipe extending inward from the reflux inlet in the distillation column; an inclined baffle positioned at a height between the reflux pipe and an upper end of the dividing wall; and a second guide baffle disposed spaced apart from the dividing wall and the first guide baffle and extending downward from one end of the inclined baffle to be adjacent to the bottom of the distillation column.

[0040] In addition, the inclined baffle may include one end positioned above the first region, the other end positioned above the second region, and the other end positioned relatively higher than the one end.

[0041] Hereinafter, the purification device of the present disclosure will be described with reference to the attached drawings, but the attached drawings are exemplary and the scope of the purification device is not limited thereto.

[0042] FIG. 1 is a drawing exemplarily showing a purification device and a process flow using the same according to one embodiment of the present disclosure, and FIG. 2 is a drawing exemplarily showing a detailed structure of a bottom region (A) of a distillation column (100) according to one embodiment of the present disclosure. In addition, FIGS. 3a and 3b are drawings exemplarily showing a cross-section of a bottom region of a distillation column according to one embodiment of the present disclosure, and FIGS. 4a, 4b, and 5 are drawings exemplarily showing an embodiment in which a magnetic filter is provided in a purification device according to one embodiment of the present disclosure, and FIG. 6 is a drawing exemplarily showing an embodiment of a second guide partition (150) having an opening in a purification device according to one embodiment.

[0043] Referring to FIG. 1, a purification device according to one embodiment of the present disclosure 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 disclosure.

[0044] A purification device according to one embodiment of the present disclosure 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.

[0045] 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.

[0046] Referring to FIG. 1, the interior of the distillation tower (100) can be divided into a bottom region (A), a middle region (B), and a top region (C).

[0047] In this specification, the term “bottom region (A)” 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 (120).

[0048] In addition, the term “top region (C)” 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.

[0049] In addition, in this specification, “middle region (B)” 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 lowest tray (120) and the uppermost tray.

[0050] In this specification, the bottom region (A), top region (C), and middle region (B) of the distillation column may be used as relative concepts. The lower part of the distillation column (100) is included in the bottom region, the upper part of the distillation column (100) is included in the top region, and unless specifically defined otherwise in this specification, the bottom region (A) is used with the same meaning as the lower region, the top region (C) is used with the same meaning as the upper region, and the middle region (B) is used with the same meaning as the side region.

[0051] In addition, inside the bottom region (A) of the distillation tower (100), a separating wall (110) is provided that extends from the bottom of the distillation tower to a predetermined height in a sump where a liquid substance to be purified is collected, and the sump region is divided into a first region (D1) and a second region (D2) with the separating wall (110) in between.

[0052] In this specification, “sump” may be used with the same meaning as the top bottom region (A). In addition, the top bottom region (A) may be divided into a liquid region and a gaseous region based on the liquid surface of the solution.

[0053] 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 may be provided so as not to be in contact with the lowermost tray (120) to be described later. Here, the predetermined height may mean a height at which the dividing wall (110) is spaced apart from the lowermost tray (120). 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 vapor in the gas phase region of the bottom region (A) can move between the first region (D1) and the second region (D2). More specifically, it is preferable that the upper end of the dividing wall (110) be located relatively lower than the height at which the reflux inlet (104) and the reflux pipe (104a) to be described later are located.

[0054] Depending on the rate at which the mineral precipitates in the first region (D1), the volume of the first region (D1) can be determined. Referring to Fig. 4b, the solution overflowing from the first region (D1) to the second region (D2) can be level controlled to prevent it from flowing back into the first region (D1).

[0055] In conventional purification equipment, the distillation column sump (lower region) typically has no dividing wall, so the section where the feed, which is the material to be purified, flows in and the bottom discharge stream (reboiler section) that is circulated to the reboiler for gas-liquid separation are not separated from each other but coexist. In this case, the bottom discharge stream supplied to the reboiler passes through the reboiler while containing inorganic substances. If inorganic substances flow into the reboiler in this way, the problem of inorganic substances accumulating in the reboiler may occur. Furthermore, the inorganic substances may be entrained in the gaseous stream of the reflux stream of the gas-liquid mixture that has passed through the reboiler and move upward, which may cause the problem of lowering the purity of the purified product.

[0056] In order to solve such a problem, the present disclosure 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 substance 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 substance content introduced into the lower discharge stream circulated to the reboiler (200).

[0057] In addition, the solution inside the second region (D2) experiences a vertical mixed flow due to the lower discharge stream of the second region (D2) and the liquid reflux stream flowing into the second region (D2). However, 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 separation wall (110) located between the first region (D1) and the second region (D2), so that relatively high-density inorganic substances can be precipitated at the bottom of the first region (D1). At this time, the precipitated inorganic substances can be discharged together with high-boiling-point organic substances through the first discharge port (102) described later.

[0058] In a purification device according to one embodiment of the present disclosure, referring to FIG. 1, a distillation column (100) may be provided with a feed supply port (101) in a middle region (B), first and second discharge ports (102, 103) and a reflux inlet (104) in a bottom region (A), and a third discharge port (105) in a top region (C).

[0059] 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. 1, 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.

[0060] The purification target material included in the above feed stream is an organic material that can be purchased as a commercially available material or manufactured by a method conventional in the field. At this time, the purification target material may contain an inorganic material as an impurity in an amount of more than 0 ppb and less than or equal to 100 ppb based on the total weight thereof. For example, the inorganic material may include one or more metal components selected from Al, As, Fe, B, Cr, Cd, Ti, Zn, and Mg. The type and content of the impurities included in the feed stream may vary depending on various environments accompanying the reaction and purification processes.

[0061] In order to remove inorganic substances contained in the above-mentioned target material for purification, the present disclosure provides a purification device capable of recovering a highly purified product by improving the structure of the bottom region (A) of the distillation column and providing additional equipment. In the distillation column (100) according to the present disclosure, the remaining structure other than the bottom region (A) can be applied without any particular limitation to the structure of a distillation column generally used in petrochemical processes, and thus a detailed description thereof will be omitted.

[0062] 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.

[0063] 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. Here, the “number of theoretical plates” refers to a virtual area in which two phases, such as gas and liquid phases, are in dynamic equilibrium with each other in the distillation column (100), or the number of stages partitioned by a plurality of trays.

[0064] Meanwhile, a purification device according to one embodiment of the present disclosure is provided with a first guide baffle (130) that extends downward from one end of the lowermost tray (120), which corresponds to a collector tray among the plurality of trays, to the upper portion of the first region (D1) and is adjacent to the bottom of the distillation column.

[0065] Referring to Fig. 2, one end of the lowermost tray (120) is open so as not to come into contact with the side of the distillation tower (100) on the first region (D1). Here, a descending liquid stream among the feed streams containing the substance to be purified can be introduced into the first region (D1) through the first guide partition (130).

[0066] In addition, as shown in FIG. 2 and FIG. 3b, the first region (D1) can be divided into a first-first region (D1-1), a first-second region (D1-2), and a first-third region (D1-3) by the first guide partition wall (130) and the second guide partition wall (150) described later.

[0067] Conventionally, the lower end of the guide baffle connected to the lowest tray is typically positioned above the liquid surface within the sump. This structure maintains the inorganic content in the solution dropped into the bottom region, while maintaining active flow within the sump, preventing the precipitation of inorganic matter.

[0068] On the other hand, in the present disclosure, the lower end of the first guide partition (130) is positioned below the liquid surface of the solution in the first region (D1), thereby inducing precipitation of a relatively dense inorganic substance, and separating the region 1-1 (D1-1) into which the descending liquid stream among the feed streams flows and the region where the inorganic substance in the solution is precipitated.

[0069] In addition, the lower end of the first guide partition (130) is positioned below the upper end of the separation wall (110), for example, the liquid level of the solution containing the substance to be purified in the first region (D1) during the purification process. More specifically, the lower end of the first guide partition (130) may be positioned adjacent to the bottom of the distillation column (100).

[0070] The height (h1) from the bottom of the distillation tower (100) to the lower end of the first guide bulkhead (130) can be determined according to the sedimentation rate of the inorganic matter, and more specifically, it is preferable to satisfy the following equation (1).

[0071] Equation (1): 0.5d1≤ h1≤ 1.5d1

[0072] In the above equation (1), d1 is the maximum gap opened between one end of the lowermost tray (120) and the inner wall (100a) of the side of the distillation column, and h1 is the height from the bottom of the distillation column (100) to the lower end of the first guide partition (130) (see FIGS. 2 and 3a). Here, d1 can be determined according to the flow rate of the solution descending from the lowermost tray (120), and for example, the larger the flow rate of the solution descending from the lowermost tray (120), the larger d1 becomes. Can be.

[0073] When the height (h1) from the bottom of the distillation column to the lower end of the first guide baffle satisfies the range of the above equation (1), the influence of the solution flow within the 1-3 region (D1-3) that receives the solution to be transferred to the 2nd region (D2) on the flow moving from the 1-1 region (D1-1) to the 1-3 region (D1-3) can be minimized. That is, the flow moving from the 1-1 region (D1-1) to the 1-3 region (D1-3) can be maintained in a state as calm as possible, thereby suppressing the mixing flow of the solutions within the 1-2 region (D1-2) and the 1-3 region (D1-3), thereby inducing the precipitation of inorganic substances.

[0074] Specifically, referring to FIG. 2, a liquid stream descending from the feed stream flows into the 1-1 region (D1-1), and then a flow is generated that moves to the 1-2 region (D1-2) and the 1-3 region (D1-3) through a space formed between the bottom of the distillation column and the first guide partition wall (130). At this time, the influence of the solution flow dropped to the 1-1 region (D1-1) by the first guide partition wall (130) on the solution in the 1-2 region (D1-2) and the 1-3 region (D1-3) can be minimized. Accordingly, precipitation of a relatively high-density inorganic substance can occur at the bottom of the 1-1 region (D1).

[0075] Furthermore, the precipitated inorganic matter is discharged as a lower discharge stream of the first region (D1), and when the liquid stream flows in to exceed the internal capacity of the first region (D1), the solution in the upper portion of the first-third region (D1-3) with minimized inorganic matter overflows and flows into the second region (D2). Accordingly, the inorganic matter in the lower discharge stream of the second region circulated to the reboiler (200) is minimized, and the entrainment of inorganic matter in the reflux stream of the gaseous phase passing through the reboiler is minimized, thereby further improving the purity of the purified product.

[0076] 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 and inorganic substances.

[0077] In the first region (D1), a descending liquid stream from among the feed streams containing the material to be purified flows into the first region (D1) through the first guide partition (130), and the solution flowing into the first region (D1) contains high-boiling-point organic substances and inorganic substances. Some 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 relatively calm solution flow is formed inside the 1-3 region (D1-3), so that inorganic substances are precipitated downward, and thus, most of the inorganic substances are included in the lower discharge stream of the first region (D1) and can be discharged through the first discharge port (102).

[0078] Meanwhile, as illustrated in FIG. 4b, the flow rate of the lower discharge stream of the first region (D1) can be controlled using a level control valve. 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).

[0079] The second discharge port (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 within the second region (D2) is discharged through the second discharge port (103), passes through the reboiler (200), and is then recycled through the reflux inlet (104) described later.

[0080] 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 upper end of the dividing wall (110). 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. Among the refluxed gas-liquid mixed phase stream, the liquid phase stream moves downward, and the vapor phase stream moves to the upper middle region (B) to undergo a gas-liquid separation process. At this time, the mass fraction of the vapor stream among the refluxed gas-liquid mixed phase stream may be 0.05 to 0.3 (i.e., 5% to 30%).

[0081] Referring to FIGS. 2 and 3b, the reflux inlet (104) is provided with a reflux pipe (104a) extending inwardly of the distillation column. The reflux pipe (104a) may be provided in a horizontal direction based on the floor. The liquid phase flow moving downward among the gas-liquid mixed phase stream refluxed through the reflux pipe (104a) is induced to descend adjacent to the inclined baffle (140) described later, thereby minimizing the liquid phase stream refluxed from the reboiler (200) from directly flowing into the second region (D2) and inducing it to flow into the first-second region (D1-2).

[0082] As shown in FIGS. 2 and 3b, a slop baffle (140) and a second guide partition (150) are provided in the bottom region (A) of the distillation column (100).

[0083] Referring to FIGS. 2 and 3b, 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). Specifically, the inclined baffle (140) may be positioned at a height between the reflux inlet (104) and the upper end of the dividing wall (110). In addition, as illustrated in FIG. 3b, a portion of the inclined baffle (140) may be in contact with the inner wall (100a) of the distillation column. The inclined baffle (140) may minimize the liquid reflux stream that has passed through the reboiler (200) from directly flowing into the second region (D2). Through this, the liquid reflux stream that has passed through the reboiler (200) can also undergo a mineral removal process once more, thereby minimizing the inflow of minerals into the second region.

[0084] 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.

[0085] According to one embodiment, as illustrated in FIG. 2, the other end of the inclined baffle positioned above the first region (D1) is positioned at a lower height than one end of the inclined baffle positioned above the second region (D2) so that the liquid reflux stream discharged from the reflux pipe (104a) can be guided to the first region (D1). Even if only a very small amount of inorganic matter is introduced into the second region (D2), the inorganic matter may accumulate in the reboiler if the purification device is continuously operated. As the process progresses, if inorganic matter accumulates in the reboiler (200), process problems such as a deterioration in product quality may occur. Therefore, it is necessary to continuously remove inorganic matter from the reflux stream that has gone through the reboiler. Accordingly, if the inclined baffle (140) is provided with a structure as illustrated in FIG. 2, the stream refluxed from the reboiler (200) can be introduced into the first region (D1), enabling additional removal of inorganic matter.

[0086] However, the reflux stream flowing in through the reflux inlet (104) and the reflux pipe (104a) has a large flow rate and a high flow rate, and when it passes to the first region (D1) through the reflux pipe (104a), it may affect the solution flow within the first region (D1), thereby hindering the smooth flow and preventing the precipitation of inorganic substances. Accordingly, the purification device according to one embodiment has a second guide partition (150) extended from the inclined baffle (140), thereby maintaining a smooth flow within the first-third region (D1-3) where the solution passing from the first region (D1) to the second region (D2) is received, thereby inducing the precipitation of inorganic substances.

[0087] Referring to FIGS. 2 and 3A, the second guide baffle (150) is spaced apart from the dividing wall (110) and the first guide baffle (130). In addition, the second guide baffle (150) may extend downward from one end of the inclined baffle (140), i.e., the end located above the first region (D1), so as to be adjacent to the bottom of the distillation column. For example, the lower end of the second guide baffle may be located relatively lower than the lower end of the first guide baffle. Through this structure, inorganic substances in the liquid stream refluxed from the reboiler (200) can be removed once again, thereby minimizing the inflow of inorganic substances into the second region (D2) and the reboiler (200), thereby improving purification efficiency and product quality.

[0088] The height (h2) from the bottom of the distillation column to the lower end of the first guide bulkhead can be determined according to the sedimentation rate of the inorganic matter, and more specifically, it is preferable to satisfy the following equation (2).

[0089] Equation (2): 0.5(d1+d2) ≤ h2≤ 1.5(d1+d2)

[0090] In the above equation (2), d1 is the maximum gap opened between one end of the lowermost tray (120) and the inner wall (100a) of the side of the distillation column, d2 is the distance between the first guide partition (130) and the second guide partition (150), and h2 is the height from the bottom of the distillation column (100) to the lower end of the second guide partition (150) (see FIGS. 2 and 3a). Here, the distance (d2) between the first guide partition (130) and the second guide partition (150) can be determined depending on the flow rate of the liquid stream refluxed from the reboiler (200). For example, d2 can increase as the flow rate of the liquid stream refluxed from the reboiler (200) increases. In addition, the distance (d3) at which the separating wall (110) and the second guide partition wall (150) are spaced apart can be determined according to the flow rate overflowing from the first region (D1) to the second region (D2). Specifically, the flow rate is the sum of the flow rate flowing in from the lowest tray (130) and the flow rate of the liquid phase refluxed after passing through the reboiler (200), minus the flow rate discharged through the first outlet (102), and the flow rate overflows from the first region (D1) to the second region (D2). The distance (d3) at which the separating wall (110) and the second guide partition wall (150) are spaced apart can be determined according to the flow rate.

[0091] In addition, by satisfying the range of the above equation (2), the liquid stream flowing back from the reboiler (200) and flowing into the first-second region (D1-2) does not overflow into the second region (D2) and can induce precipitation of inorganic substances within the first-second region (D1-2).

[0092] In addition, when the flow rate of the liquid stream refluxed from the reboiler (200) is large and d2 is more than twice d1, the flow rate of the liquid moving from the 1-2 region (D1-2) to the 1-3 region (D1-3) through the space between the lower end of the second guide partition (150) and the bottom of the distillation column (100) may increase. In this case, in order to lower the flow rate at the bottom of the first region (D1), as illustrated in FIG. 6, one or more openings (151) may be provided at a position adjacent to the lower end of the second guide partition (150). When one or more openings (151) are provided at the bottom of the second guide partition (150), the flow rate of the liquid flowing into the space spaced between the lower end of the second guide partition (150) and the bottom of the distillation column (100) can be reduced, thereby minimizing the influence of mineral precipitation at the bottom of the first region (D1).

[0093] The number and size of the openings (151) provided in the second guide partition wall can be appropriately designed and changed depending on the flow rate of the liquid stream flowing into the first-second region (D1-2) or the flow rate of the liquid moving from the first-second region (D1-2) to the first-third region (D1-3) through the space between the lower end of the second guide partition wall (150) and the bottom of the distillation column (100).

[0094] Meanwhile, in accordance with one embodiment, a purification device may further include, with reference to FIGS. 4A and 4B, a magnetic filter (300) for removing inorganic substances in at least one of an inlet pipe connected to the feed supply port (101) and an outlet pipe connected to the first outlet (102). More specifically, the magnetic filter (300) may be provided inside a strainer installed in the pipe to filter out foreign substances in the fluid. When the magnetic filter (300) is provided, the removal efficiency of inorganic substances (metals) having magnetism, such as iron (Fe) and magnetite, can be further improved. When the magnet is provided in the inlet pipe and / or the outlet pipe rather than inside the distillation column, maintenance of the device can be easier. In particular, as shown in FIG. 4a, when a magnetic filter (300) is provided in the shear pipe, it may be more preferable in that inorganic substances in the feed stream can be primarily removed before being supplied to the distillation tower (200).

[0095] Furthermore, a pump (400) for transporting a solution (feed stream or lower discharge stream of the first region) is provided in the front pipe and / or the back pipe of the distillation tower. Since a malfunction may occur if foreign substances are introduced into the pump, a strainer equipped with a magnetic filter (300) is provided in front of the pump (400) to prevent foreign substances from being introduced into the pump.

[0096] According to one embodiment, as shown in FIG. 5, a pipe branched in a parallel structure is provided for maintenance of the pump (400a, 400b), and a magnetic filter (300a, 300b) and a pump (400a, 400b) can be installed in each of the pipes branched in the parallel structure.

[0097] For example, the shear pipe connected to the feed supply port (101) may include a branch into a first shear pipe and a second shear pipe, as illustrated in FIG. 5. At this time, a magnetic filter (300a, 300b) may be installed in each of the first shear pipe and the second shear pipe, and furthermore, a pump (400a, 400b) for transporting the solution may be further provided. In this case, when the feed is supplied, the pump (400a) provided in one of the first shear pipe and the second shear pipe is operated, and the pump (400b) provided in the remaining pipe is in a standby state to proceed with the process, and when a problem occurs in the pump (400a) being used, the operation may be switched to the pump (400b) in the standby state.

[0098] In detail, one of the first pre-stage pipe and the second pre-stage pipe may be in an idle state, and the magnetic filter and pump provided in the idle state pipe can be maintained. For example, if impurities accumulate in the first pre-stage pipe or the magnetic filter (300a) and / or pump (400a) provided therein in an operating state or a malfunction occurs, the first pre-stage pipe is switched to an idle state and then maintenance is performed, and at the same time, a feed stream is supplied to the second pre-stage pipe, so that the continuous operation of the purification device can be enabled by the magnetic filter (300b) and / or pump (400b) provided in the second rear-stage pipe.

[0099] As another example, the downstream pipe connected to the first outlet (102) may include a branching into a first downstream pipe and a second downstream pipe, as illustrated in FIG. 5. At this time, a magnetic filter (300a, 300b) may be installed in each of the first downstream pipe and the second downstream pipe, and a pump (400a, 400b) for transporting the solution may be further provided. At this time, the first downstream pipe and the second downstream pipe may be switched and operated for maintenance.

[0100] In detail, one of the first rear-end pipe and the second rear-end pipe may be in an idle state, and the magnetic filter and pump provided in the idle pipe may undergo maintenance. For example, if impurities accumulate or a malfunction occurs in the first rear-end pipe or the magnetic filter (300a) and / or pump (400a) provided therein in an operating state, the first rear-end pipe may be switched to an idle state and then maintenance may be performed, and at the same time, a feed stream may be supplied to the second rear-end pipe, so that the purification device may be continuously operated by the magnetic filter (300b) and / or pump (400b) provided in the second rear-end pipe.

[0101] According to one embodiment, a third outlet (105) may be located in the top region (C) of the distillation column. For example, products and / or low-boiling-point organic substances included in the material to be purified may be discharged through the third outlet (105).

[0102] 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).

[0103] For example, the material to be purified supplied to the distillation tower (100) undergoes a separation process by continuous gas-liquid contact in each stage included in the intermediate region (B), and relatively low-boiling-point organic substances and products 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 can be discharged through the first outlet (102) of the bottom region (A). Furthermore, the effluent from the top region (C) can undergo an additional purification process as needed, through which a high-purity product can be ultimately obtained.

[0104] The purification device according to one embodiment of the present disclosure may additionally include devices such as a condenser, a reboiler, a valve, a pump, and a separator, as needed.

[0105] Above, the purification device according to the present disclosure 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 disclosure, 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 disclosure.

[0106] Although exemplary embodiments of the present disclosure have been described above, the present disclosure 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.

[0107] [Explanation of symbols]

[0108] 100: Distillation tower

[0109] A: Top-bottom area

[0110] B: Middle area

[0111] C: Top area

[0112] D1: Area 1

[0113] D1-1: Area 1-1

[0114] D1-2: Area 1-2

[0115] D1-3: Area 1-3

[0116] D2: Area 2

[0117] 101: Feed supply port

[0118] 102: First outlet

[0119] 103: Second outlet

[0120] 104: Reflux inlet

[0121] 104a: Reflux pipe

[0122] 110: Separation wall

[0123] 120: Bottom tray

[0124] 130: 1st guide bulkhead

[0125] 140: Inclined baffle

[0126] 150: Second guide bulkhead

[0127] 151: Aperture

[0128] 200: Re-Bicycle

[0129] 300, 300a, 300b: Magnetic filter

[0130] 400, 400a, 400b: Pump

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 middle region of the distillation column is provided with a feed supply port provided on one side of the middle region for supplying a feed stream containing a substance to be purified to the distillation column; and a plurality of trays spaced apart from each other in the middle region; The bottom region of the distillation column includes a first region and a second region, which are separated by a dividing wall extending from the bottom of the distillation column to have a predetermined height therein; a first guide partition wall disposed spaced apart from the dividing wall in the first region and extending downward from one end of the lowest tray to be adjacent to the bottom of 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; a reflux inlet port provided at an upper portion of the second region and connected to the other side of the reboiler; a reflux pipe extending inwardly of the distillation column from the reflux inlet port; an inclined baffle positioned at a height between the reflux pipe and an upper end of the dividing wall; and a second guide partition wall disposed spaced apart from the dividing wall and the first guide partition and extending downward from one end of the inclined baffle to be adjacent to the bottom of the distillation column. A purification device, comprising: one end of the inclined baffle is positioned above the first region, the other end is positioned above the second region, and the other end is positioned relatively higher than the one end.

2. In paragraph 1, A purification device comprising a magnetic filter provided in at least one of an inlet pipe connected to the feed supply port and an outlet pipe connected to the first discharge port.

3. In paragraph 2, The shear pipe connected to the above feed supply port includes a branch into a first shear pipe and a second shear pipe, A purification device, wherein the magnetic filter is provided in each of the first shear pipe and the second shear pipe.

4. In paragraph 2, The rear pipe connected to the first outlet is branched into a first rear pipe and a second rear pipe, A purification device, wherein the magnetic filter is provided in each of the first rear pipe and the second rear pipe.

5. 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.

6. In paragraph 5, 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.

7. In paragraph 5, A feed stream containing the material to be purified is introduced into the first region through the first 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.

8. In paragraph 1, The height (h1) from the bottom of the distillation column to the lower end of the first guide bulkhead satisfies the following equation (1): Equation (1): 0.5d1≤ h1≤ 1.5d1 In the above equation (1), d1 is the maximum open gap between one end of the lowermost tray and the side of the distillation column, and h1 is the height from the bottom of the distillation column to the lower end of the first guide baffle.

9. In paragraph 1, The height (h2) from the bottom of the distillation column to the lower end of the first guide bulkhead satisfies the following equation (2): Equation (2): 0.5(d1+d2) ≤ h2≤ 1.5(d1+d2) In the above equation (2), d1 is the maximum open gap between one end of the lowermost tray and the side of the distillation column, d2 is the separation distance between the first guide baffle and the second guide baffle, and h2 is the height from the bottom of the distillation column to the lower end of the second guide baffle.

10. In paragraph 1, A purification device having one or more openings located adjacent to the lower end of the second guide bulkhead.

Images