JP2016107181A - Distillation tower filled with filler - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a distillation tower directly used without needing any filling work of a filler.SOLUTION: The distillation tower used for a distillation method includes a distillation tower 1 having a cylindrical fractionation part 10 of desired diameter and length, and a filler 2 including a metal coil body 20 formed by curling a metal thin wire made of flat stainless steel in a coil shape. The fractionation part is filled with the filler by a desired density to form the distillation tower filled with the filler. The cylindrical fractionation part is formed into a cylindrical shape or a circular tube shape. As the fractionation part is filled with the filler by the desired density, the standardized high-performance distillation tower can be provided to be directly used by a user.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a distillation column used in a distillation method. More specifically, the present invention relates to a distillation column packed with a packing used for separating components by heating and evaporating a liquid mixture of a plurality of components.

  Conventionally, a large number of operations such as distillation and fractional distillation have been carried out in academic research relating to chemistry, chemical industry, pharmacy, and business.

  As the distillation method, for example, a filling type in which a packing is filled in a distillation column or fractionation column (or fractionation tube), and a multistage type in which shielding plates and shelves are arranged in multiple stages in the distillation column etc. (Also referred to as a step type) is generally widely known. The present invention relates to a distillation column used in a packed distillation method.

  The packed distillation method is performed, for example, by the following method. Hereinafter, an outline of the example will be described with reference to FIG. FIG. 4 is an explanatory view schematically showing a configuration of an example distillation apparatus 5 used in a packed distillation method and a method of using the same. In the figure, 50 is a distillation column (or fractionation column or fractionation tube), 51 is a distillation kettle connected to a joint plug 50a (male joint) at the lower end of the distillation column 50, and 52 is a monoheat (mantle heater). , 53 is a temperature controller, 54 is a cooler (condenser) disposed at its upper end connected to a joint port pipe 50b (female joint) at the upper end (top) of the tower 50 by a connecting pipe 55, 56 is a cooler 54 A receiver (collecting container) 57 connected to the lower end, 57 indicates an open / close cock interposed in an outflow pipe 58 protruding from the lower end of the receiver 55.

  Accordingly, the packed material 6 is filled in the distillation column 50 (in the cylindrical fraction 50c of the column 50) and the liquid mixture 7 (solution) to be distilled (distilled) is sealed in the kettle 51. When the kettle 51 is heated by the heater 52, the solution distills (vaporizes) and enters the column 50, and rises in the column 50 while being in contact with the packing 6; Heat exchange is effected by contact, and the component having a high boiling point liquefies and adheres to the packing, and the component having a low boiling point rises as it is because it does not liquefy.

  As described above, while the steam (mixed steam) heated and distilled rises in the column 50, it is in contact with the packing 6 and the liquid liquefied and adhering to the packing to exchange heat. In the middle of the process, it liquefies and flows down, is refluxed into the kettle 51, and the low-boiling component rises in a vaporized state and is introduced into the cooler 54 through the connecting pipe 55. Then, it is liquefied (condensed) in the cooler 54 and collected in the receiver 56. As described above, the solution 7 (liquid mixture) in the pot 51 is separated and separated according to the boiling point of the components. The distillation apparatus 5 is disclosed as an example as described above.

  Conventionally, various packing materials used in the distillation method are generally known, such as a spherical shape (glass sphere), a ceramic tube (cylindrical shape), and a McMahon. These fillers are appropriately selected and used in accordance with the type and application of the components of the target liquid mixture (solution).

  By the way, as one of the important criteria for determining whether the packing performance is good or bad, the surface area of the packing filled per unit volume is larger or smaller.

  Therefore, looking at the conventional example illustrated above, first, the spherical glass sphere (conventional example 1) has the smallest surface area compared to other shapes. In this case, if the sphere is formed to be porous, the surface area increases, but it is difficult to manufacture a large number of small holes in a small glass sphere (diameter of about 3 to 5 mm).

  Next, the ceramic pipe (conventional example 2) is made by cutting a ceramic pipe material having a small diameter (for example, an outer diameter of about 3 to 5 mm), and the surface area is somewhat larger than the glass sphere of the conventional example 1, Still small other than that.

  Next, McMahon (Conventional Example 3) is formed by bending a stainless steel net having a width of about 6 mm into a substantially U shape, and its surface area is somewhat larger than the cylindrical shape (ceramic pipe) of Conventional Example 2. However, there is not much difference.

  As described above, the fillers of Conventional Examples 1 to 3 have the problems described above. Then, this inventor repeated the research and experiment in order to eliminate the above-mentioned problem which the conventional example has, and as a result, the packing material (prior art) described in JP 2011-125841 A (Patent Document 1) was obtained. developed.

  As disclosed in the above-mentioned publication, the above prior art filler is composed of a metal coiled body formed by curling a thin metal wire made of flat stainless steel or the like into a coil shape.

  According to the prior art packing, the surface area is greatly increased, which can greatly increase the contact surface of gas and liquid, thus improving the performance compared with the conventional examples 1 to 3, and exhibiting an excellent fractionation effect Can be made. Moreover, the packing which reduced the production cost can be provided. In addition, the said effect has become clear as a result of experiment.

JP 2011-125841 A

  According to the prior art packing, it is possible to provide a packing that exhibits excellent operational effects as described above. However, the following problems remain in the prior art.

  The packing is appropriately loosened and packed into a distillation column (or fractionation column or fractionation tube). However, since the filler is composed of a metal coil-like body, it tends to be entangled, which may make it difficult to unravel. Therefore, it takes time to fill the distillation column.

  In addition to the above, the packing has a large or small difference in performance depending on the packing density in the column. Therefore, the packing density becomes an important condition. It is also important to fill so that there is no uneven filling. However, as described above, since the filling is easy to get entangled, it takes a lot of work and skill to fill the filling so as to obtain a desired filling density and non-uniform filling. In particular, as in a distillation column used in an experimental apparatus, for example, the packing is placed in a small-diameter distillation column such as a column inner diameter of about 15 mm to about 25 mm and a length of about 100 mm to about 600 mm. It is extremely difficult to perform filling so as not to have a desired filling density and filling unevenness.

  Therefore, in view of the above situation, the present invention can utilize the features of the prior art packing as it is, exhibit excellent performance (fractionation effect), and can be used as it is without requiring a filling operation. An object is to provide a distillation column.

In order to achieve the above object, the present invention is a distillation column used in a distillation method,
A distillation column having a cylindrical fraction with a desired diameter and length;
A filling made of a metal coiled body formed by curling flat metal fine wires into a coil shape,
The cylindrical packing fraction is filled with the packing material at a desired density, and is characterized in that it is configured.

  In the present invention, the term “coiled” is used as a concept including the meaning of “spiral”. Further, the term “metal coil-like body” is used as a concept including a “metal spiral body” formed by curling in a spiral shape. Furthermore, the term “distillation column” is used as a concept including “fractionation column” and “fractionation tube”.

  In the present invention, the metal thin wire may employ a configuration employing a stainless steel thin wire.

  In the present invention, it is possible to adopt a configuration in which the cylindrical packed portion of the distillation column is formed in a substantially cylindrical shape or a substantially circular tube shape.

According to the present invention, the following operational effects can be obtained.
(1) Since the packing is composed of a metal coiled body formed by curling flat metal fine wires into a coil shape, the surface area of the packing is greatly increased, thereby reducing the contact surface of gas and liquid. Can increase significantly. Therefore, a packing exhibiting extremely excellent performance (fractionation effect) can be obtained.
(2) The packing is packed at a desired density in the cylindrical packing section of the distillation column. Therefore, the user of the distillation column can use the purchased distillation column as it is without requiring the work of filling the packing.
(3) It is possible to provide a high-performance standardized distillation column by setting the packing density of the packing to a predetermined density.

BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows schematically the structure of the distillation column filled with the packing of one Embodiment of this invention, Comprising: The same figure (a) is an explanatory longitudinal cross-sectional view, The same figure (b) is A of the same figure (a). FIG. FIG. 2 (a) is an explanatory perspective view schematically showing the structure of a wire mesh member provided on the upper end side of the distillation column, and FIG. 2 (b) is a schematic view of the structure of the wire mesh member provided on the lower end side. FIG. It is an explanatory perspective view which expands a part of packing constituted with a metal coil-like object, and shows the composition roughly. It is explanatory drawing which shows roughly the structure of the example distillation apparatus used for the filling-type distillation method, and its usage method.

  Hereinafter, an example of an embodiment of the present invention will be described with reference to the drawings.

  1 to 3 show an embodiment of the present invention. As shown in these drawings, the distillation column 100 filled with the packing according to the present embodiment includes a distillation column 1 and a packing 2 filled in the distillation column 1.

  The distillation column 1 of this embodiment includes a cylindrical fraction 10 having a desired diameter and length, and a joint port 11 (female joint) provided integrally with the upper end opening in FIG. And a joint plug 12 with both ends opened integrally with the lower end opening of the fractionator 10. The fractionation part 10 of this embodiment is formed in a substantially cylindrical shape or a substantially circular tube shape.

  The distillation column 1 of the embodiment includes a conical metal mesh member 13 for receiving a packing provided at the lower end opening of the fractionation unit 10 and a metal mesh member 14 for holding a filler provided at the upper end opening of the fractionation unit 10. With.

  The diameter and length of the fractionation section 10 of the distillation column 1 (height for filling the packing material) are not particularly limited and are set as desired. For example, the inner diameter is about 15 mm to about 15 mm. 30 mm, length: about 100 mm to about 800 mm can be mentioned. However, it is not limited to the above range.

  The distillation column 1 is made of, for example, transparent glass having heat resistance. Further, the inner peripheral wall surface of the joint port tube 11 and the outer peripheral wall surface of the joint plug 12 are polished by sliding or the like.

  As shown in detail in FIG. 3, the filler 2 is composed of a metal coil-like body 20 formed by curling (curling) a flat metal fine wire 21 in a coil shape or a spiral shape.

  The metal thin wire 21 of this embodiment is composed of a stainless steel thin wire. The thickness and width of the thin metal wire 21 are not particularly limited, and examples thereof include a thickness range of about 0.005 mm to about 0.01 mm and a width of about 0.3 mm to about 1.5 mm. . However, the present invention is not limited to the above range.

  The diameter of the metal coil-shaped body 20 is not particularly limited, and examples thereof include a range of about 2 mm to about 5 mm in diameter (outer diameter). However, it is not limited to the above range. The length of the metal coil-shaped body 20 is not particularly limited, and can be arbitrarily determined as desired. For example, the length of the metal coil-shaped body can be in the range of about 5 mm to about 10 m (meters). However, it is not limited to the above range, and can be formed to a length of 5 mm or less, or 10 meters or more.

  The metal thin wire 21 can be formed by crushing a metal round wire (in this embodiment, a stainless steel round wire) having a diameter of about 0.1 mm to about 0.3 mm and processing it into a flat shape. In this case, if necessary, the round wire is crushed while being drawn and processed into a flat shape. The metal coil-shaped body 20 is formed by curling (curling) the metal thin wire 21 (flat metal thin wire) processed into a flat shape as described above into a coil shape or a spiral shape. In addition, the diameter of the stainless steel round wire which comprises the said thin wire 21 was mentioned as an example, and is not limited to the said range.

  The flat metal thin wire 21 and the metal coil-like body 20 can be manufactured, for example, by a manufacturing method similar to a conventionally known “metal scrubbing”. As shown in FIG. 3, the metal coil-shaped body 20 may be formed by curling the adjacent curled portions 21a in contact with each other in a coil spring shape, or between the curled portions 21a as shown in FIG. As shown, a desired gap 21b may be formed and curled.

  The distillation column 100 of the present embodiment is configured by filling the packing 2 with a desired density (packing density) in the fractionation unit 10 of the distillation column 1. Specifically, a conical wire mesh member 13 is attached to the lower end opening of the fractionator 10. Then, the filler 2 is pushed into the fractionation unit 10 from the joint mouth tube 11 of the distillation column so as not to cause uneven filling, and is packed to a desired density, and the presser wire mesh member 14 is inserted into the upper end opening of the fractionation unit. And the upper surface of the filling layer of the filling 2 is pressed.

  By the way, as described above, the packing 2 has a difference in performance (fractionation effect) depending on the packing density. Therefore, the density is set and filled so as to exhibit excellent performance.

  Therefore, as a result of experiments using the distillation column 100 packed with the packing material of the present embodiment, the present inventor has found a packing density that exhibits extremely excellent performance. Evaluation of the performance of the distillation column was made by measuring the number of theoretical plates using the Fengke equation, and the packing height per one theoretical plate (height of the fractionation section). E. T.A. P. Judged by (Height Equivalent to a Theoretical Plate) (mm / stage).

In this experimental example, a distillation apparatus equipped with a 500 ml distillation kettle is used for the following three types of distillation columns, and n-heptane and methylcyclohexane (relative volatility α = 1.075) are used as measurement reagents. Was carried out.
Specifically, 75 ml each of n-heptane and methylcyclohexane (150 ml in total) were charged, and after about 1 hour from the start of heating and refluxing, it was confirmed that the column top temperature was stable. A sample solution was collected from (the top of the distillation column), each composition was calculated with a gas chromatograph analyzer, and the number of theoretical plates was calculated using Fenske's equation. Further, the height of each distillation column (the length of the fractionation section) is divided by the number of the above stages to obtain an H.P. E. T. T. et al. P. Asked. H. E. T. T. et al. P. The smaller the value, the better the distillation efficiency. The experiment was performed three times for each distillation column. The measurement results are shown in Table 1 below. In the table below, the number of theoretical plates and the H.P. E. T. T. et al. P. The numerical value of shows the average value of 3 times each.

(Distillation tower size)
(1) Example 1 ... Inner diameter: 16 mm, Length of fractionation part (filling height, the same applies hereinafter): 100 mm
(2) Example 2 ... Inner diameter: 16 mm, Length of fractionation part 150 mm
(3) Example 3... Inner diameter: 16 mm, Length of fractionated part 200 mm

  In Table 1, each of the distillation columns of Examples 1 to 3 is packed in a coil shape with a stainless steel wire having a wall thickness of about 0.008 mm and a width of about 0.5 mm as a packing. A metal coil-shaped body formed by curling was used.

  As is apparent from Table 1 above, each of the distillation columns of Examples 1, 2, and 3 has an extremely excellent performance (fractionation effect) by being configured by filling the packing with a density of 0.6 g / cc. It was found that

  In addition, as a result of experimenting by changing the packing density of the packing, when the density is 0.6 g / cc or less, the numerical value of the theoretical plate becomes proportionally smaller. E. T.A. P. It has been found that the performance of the distillation column deteriorates, especially when the value is 0.5 g / cc or less, so that the performance is extremely lowered. On the contrary, if the density is 0.6 g / cc or more, the numerical value of the theoretical plate number increases, but if the density is increased too much, the problem of pressure loss occurs and the efficiency decreases. Therefore, the packing density of the packing is preferably set in the range of about 0.55 g / cc to about 0.62 g / cc. In addition, it becomes impossible to fill the density to about 0.65 or more, and it becomes almost impossible.

  Moreover, when this inventor experimented by the method similar to the above using the distillation column which differed in size from the three types of distillation columns mentioned above, it turned out that the same result as the above was obtained.

  The distillation column packed with the packing of the present embodiment is used as it is in the past by incorporating it into a distillation apparatus as it is.

  According to this embodiment, it is possible to provide a high-performance standardized distillation column by configuring the packed distillation column with the packing density set to a predetermined packing density.

  The distillation column of the above-described embodiment is disclosed as an example, and the present invention is not limited to the above-described embodiment, and is arbitrarily changed within the scope not departing from the technical idea described in the claims. It is possible.

DESCRIPTION OF SYMBOLS 1 Distillation column 2 Packing material 10 Tubular fractionation part 20 Metal coil-shaped body 21 Metal fine wire

Claims (3)

A distillation column used in a distillation method,
A distillation column having a cylindrical fraction with a desired diameter and length;
A filling made of a metal coiled body formed by curling flat metal fine wires into a coil shape,
A distillation column packed with a packing, wherein the packing is packed with a desired density into the cylindrical fraction.   The distillation column filled with packing according to claim 1, wherein the metal fine wire is a stainless steel fine wire.   The distillation column packed with a packing material according to claim 1, wherein the cylindrical fractionation part is formed in a substantially cylindrical shape or a substantially circular tube shape.

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