WO2015026161A1

WO2015026161A1 - Method for purifying isopropyl alcohol

Info

Publication number: WO2015026161A1
Application number: PCT/KR2014/007737
Authority: WO
Inventors: 박종서; 이성규; 신준호; 이종구
Original assignee: 주식회사 엘지화학
Priority date: 2013-08-20
Filing date: 2014-08-20
Publication date: 2015-02-26

Abstract

The present application relates to a method and an apparatus for purifying isopropyl alcohol. In the present application, water can be effectively removed from a feed comprising water and isopropyl alcohol with a minimum of energy consumption, thereby allowing highly pure isopropyl alcohol to be obtained.

Description

Method for Purifying Isopropyl Alcohol

The present application relates to a method and apparatus for purifying isopropyl alcohol.

Isopropyl alcohol (hereinafter, referred to as "IPA") is used in various applications including applications such as cleaning agents in the electronic industry, such as semiconductor and liquid crystal display (LCD) manufacture, for example.

IPA can be produced using, for example, propylene or acetone as a raw material. In most cases, IPA reactants containing a large amount of water are obtained in the preparation of IPA, which forms an azeotrope containing water together. That is, the boiling point of water at about 100 ℃ and the IPA of about 82.5 ℃ to form azeotropy of IPA 87.9 wt% at an azeotropic temperature of 80.4 ℃, thus removing the water from the feed efficiently high-purity IPA It is required to manufacture and a lot of energy is consumed to remove the water by simple distillation process. As a method for obtaining high purity IPA from the azeotropic mixture, a distillation method of adding an azotropic agent, which is a substance for extracting or forming an azeotrope, is known.

The present application provides a method and apparatus for purifying IPA.

The present application relates to a method for purifying IPA. In an exemplary purification method, water is removed via a step of supplying a feed to the dewatering means D to remove water as described with reference to FIG. 1 (hereinafter referred to as a "dehydration step") and the dewatering means D. It may include a step (hereinafter referred to as "refining process") of introducing the purified feed into the purification means (P) and purification. According to the purification method of the present application, during the IPA purification process using the dehydration means (D) and the dividing wall distillation column 200, it is possible to derive the optimum operating conditions of the dividing wall distillation column to minimize the water content in the IPA product In this way, not only can the IPA be purified with high purity, but also the purification is carried out through one dividing wall distillation column, so that the efficiency is higher than in the case of using the purification means P connected with two general distillation columns. IPA can be purified.

As used herein, the term "removing water" does not mean removing 100% of the water contained in the feed, and the feed is supplied to the dehydration means (D), and the water is removed or subjected to a purification process. In other words, it means that the content of IPA is made rich. As used herein, the term "rich stream" means the content of IPA contained in the flow via the dehydration means (D) or the purification means (P) rather than the content of IPA contained in the feed before being supplied to the dehydration means (D). This higher flow means, for example, the content of IPA contained in the flow via the dehydration means (D) or the purification means (P) has a content of 50% by weight or more, 80% by weight or more, 90% by weight. It may mean a flow of at least 95% by weight or more than 99% by weight.

In one example, the feed supplied to the dewatering means D in the dewatering process may include IPA and water. The water content of the feed, ie the content of water in the feed, may be up to 5,000 ppm, for example up to 3,000 ppm, up to 2,500 ppm or up to 2,200 ppm. In addition, the lower limit of the water content in the feed may be, for example, 1,200 ppm. The water content in the feed acts as a very important factor in the efficiency of the method, and thus the water content of the feed needs to be adjusted within the above range. The feed contains IPA and water, and the specific composition is not particularly limited as long as the water content is adjusted within the above range. Typically, depending on how the feed containing the IPA is produced, various kinds of impurities may be included in the feed, and the impurities may be efficiently removed by the above method.

In the method, the dewatering means (D), for example, when a feed having a water content of 3,000 ppm is introduced, the water content in the feed is 500 ppm or less, for example, 400 ppm or 300 ppm or less through the dehydration process. It can be installed so that it can be discharged by lowering it. Accordingly, the method may include controlling the water content of the feed to 500 ppm or less, for example, 400 ppm or less or 300 ppm or less by removing water from the feed fed to the dehydration means (D).

The dewatering means (D) in which the feed is introduced in the method may comprise, for example, a column (110, 111) filled with a membrane system and an adsorbent. In one example, the dehydration process may be a two-step dehydration process, for example, the first dehydration process and the second dehydration process in sequence. The membrane system 100 and the

columns

110, 111 of the dewatering means D are fluidically connected such that an incoming feed flows through the membrane system 100 and the

columns

110, 111. The first dehydration process may be performed in the membrane system 100, and the second dehydration process may be performed in the

columns

110 and 111 filled with the adsorbent.

In the dehydration means (D), when the feed having a water content of 3,000 ppm is introduced, for example, the membrane system 100 can discharge the water content in the feed from 500 ppm to 1,200 ppm through the first dehydration process. It may be installed so that By controlling the water content in the above range through the membrane system 100 can increase the efficiency of the subsequent purification process. As used herein, the term "membrane system" means a system or device that separates a fluid using a separator.

As the membrane system 100 of the dehydration means (D), any system using a separation membrane is not particularly limited, but, for example, a pervaporation system or a vapor permeation system may be used. .

The "permeation evaporation" refers to a method of increasing the purity of the feed by supplying a liquid feed to the permeation membrane and selectively permeating a material having affinity to the membrane, and the material passing through the permeation membrane is a constant vacuum state Is evaporated and discharged from the water, which is then cooled and collected in a cooler. The pervaporation system may be preferably applied when the feed is in a liquid state in the purification method of the present application. When the dehydration process is performed using the pervaporation system, water is selectively removed in the dehydration process before the feed is introduced into the dividing wall distillation column 200, compared to the case of removing water by a simple distillation process. High purity IPA can be obtained economically.

In one example, when the dehydration means (D) comprises a pervaporation system, the introduction of the liquid feed into the pervaporation system in the dehydration process is, for example, 40 to 120 ° C, 70 to 110 ° C or 80 To 100 ° C., but is not particularly limited thereto. In addition, the introduction of the liquid feed into the pervaporation system, for example, 1.0 Kg / cm ² to 10.0 Kg / cm ² , 2.0 Kg / cm ² to 8.0 Kg / cm ² , 2.5 Kg / cm ² to 6.0 Kg / cm ² or 3.0 Kg / cm ² to 5.0 Kg / cm ² . In the temperature and / or pressure range as described above, the dehydration process of the liquid feed may be performed efficiently. However, the temperature and / or pressure range may be appropriately changed in consideration of the target dehydration amount and the kind of separation membrane used. For example, in general, as the temperature and pressure are higher, the permeability of the separator may be higher, but the upper limit of the temperature and pressure may vary depending on the type and process conditions of the separator. Although the permeate flow rate can be increased, the upper limit value may be adjusted within a specific range depending on the kind of material of the separator used and the durability of the separator.

The "vapor permeation" means a membrane separation method of vaporizing a feed to contact a gas and a separation membrane to separate a desired gas through the membrane, and in the purification method, it may be preferably applied when the feed is in a gaseous state. When the dehydration process is performed using the vapor permeation system, since the azeotropy does not appear, water can be removed more efficiently than when the dehydration process is performed by a distillation method, and thus, high purity IPA can be economically obtained.

In one example, the feed flowing into the vapor permeation system of the dewatering means (D) may be introduced into the vapor permeation system at a temperature above the boiling point of the mixed composition of water and IPA. Introduction of the gaseous feed into the vapor permeation system in the dehydration process, for example, may be carried out at a temperature of at least 90 ℃, at least 100 ℃, at least 110 ℃, at least 120 ℃ or at least 150 ℃, the introduction of the gas feed The upper limit value of the temperature may be changed depending on the thermal or chemical properties of the separator used, but is not particularly limited, but may be performed at a temperature of, for example, about 180 ° C. In addition, the introduction of the gaseous feed into the vapor permeation system is, for example, 1.0 Kg / cm ² to 10.0 Kg / cm ² 2.0 Kg / cm ² to 8.0 Kg / cm ² or 3.0 Kg / cm ² to 6.0 Kg / It can be carried out at a pressure of cm ² . In the temperature and / or pressure range as described above, the dehydration process of the gaseous feed may be efficiently performed. However, the temperature and / or pressure range may be appropriately changed in consideration of the target dehydration amount and the kind of separation membrane used.

Separation membrane that can be used in the pervaporation system or vapor permeation system may be an organic separation membrane, such as a polymer membrane, an inorganic separation membrane, an organic-inorganic separation membrane prepared by mixing organic and inorganic substances, etc. according to the type of material used, In the dehydration means (D) of the present application, various separators known in the art may be variously used depending on the desired separation component. For example, as the hydrophilic separator, a separator made of silica gel, a separator made of a polymer such as PVA or polyimide, and a zeolite separator may be used, but may be appropriately changed in consideration of the desired dehydration amount and the composition of the feed. As the zeolite membrane, a zeolite membrane of Pervatech, a zeolite A membrane of i3nanotec, a zeolite NaA membrane, etc. may be used, but is not limited thereto.

Further, the pervaporation system or vapor permeation system may comprise a vacuum device. The vacuum device means a device for forming a vacuum so that a component desired to be separated in the feed can be easily separated from the membrane after contact with the separator, and an apparatus including a vacuum storage tank and a vacuum pump may be exemplified. .

In the exemplary dewatering means D, the adsorbent-filled

columns

110, 111 pass through the membrane system 100 described above, for example, when a feed having a water content of 500 ppm to 1,200 ppm is introduced. In addition, the water content in the feed through the second dehydration process may be installed to be discharged by adjusting to 50 ppm to 500 ppm, for example, 100 ppm to 500 ppm or 150 ppm to 500 ppm. By controlling the water content in the range through the columns (110, 111) it is possible to increase the efficiency of the subsequent purification process.

In one example, various adsorbents known in the art may be used, for example, molecular sieves, silica gel, activated alumina, activated carbon, or ion exchange resins, but are not limited thereto. no.

For example, as the molecular sieve of the dehydration means (D), any known molecular sieve can be used without particular limitation as long as it is provided to have the above dehydrating ability. For example, zeolite-based molecular sieves, silica-based molecular sieves, alumina-based molecular sieves, silica-alumina-based molecular sieves, or silicate-alumina-based molecular sieves can be used.

As the molecular sieve, for example, molecular sieves having an average pore size of about 1.0 kPa to 5.0 kPa or about 2.0 kPa to 4.0 kPa can be used. In addition, the specific surface area of the molecular sieve may be, for example, about 100 m ³ / g to about 1500 m ³ / g. Through the use of molecular sieves having a pore size and specific surface area in this range, it is possible to appropriately control the dewatering ability of the dewatering means (D).

In one example, the dehydration means (D) may include two or more

such columns

110 and 111 as described above. 2 exemplarily shows a case in which two molecular sieves are filled with

columns

110 and 111. As shown in FIG. 2, when two or

more columns

110 and 111 are included in the dehydration means D and feeds are alternately supplied to the plurality of

columns

110 and 111, the efficiency of the process may be improved. It can be higher.

The method may further include regenerating the molecular sieve by desorbing water adsorbed into the molecular sieve in the dehydration process. The desorption process of the molecular sieve may be performed, for example, in the course of a dehydration process followed by a purification process, or when a plurality of

columns

110 and 111 are used as described above, any one column 110. ) May be performed on the other column 111 during the dehydration process.

The regeneration may be performed using, for example, argon, carbon dioxide or nitrogen, lower alkanes such as methane, ethane, propane or butane and the like. In one example, the regeneration process may be performed using nitrogen gas. In the case of using nitrogen gas, the regeneration process may be performed at a temperature of about 175 ° C to 320 ° C or about 180 ° C to 310 ° C. In addition, the flow rate of the nitrogen gas supplied for desorption may be adjusted, for example, about 1,100 Nm ³ / hr to 1,500 Nm ³ / hr. Regeneration or desorption process can be efficiently performed within the above range. However, the temperature and flow rate may vary depending on the type and amount of specific molecular sieve.

The feed whose water content is adjusted to 500 ppm or less through the dehydration process may be supplied to the purification means P to proceed with the purification process. In one example, the purifying means P may be a divided wall column (DWC).

The dividing wall distillation column 200 is a device designed for distillation of a feed including three components, namely low boiling point, middle boiling point and high boiling point. The dividing wall distillation column 200 is a device similar in terms of thermodynamics to a so-called Petlyuk column. In the case of a thermal complex distillation column, the preliminary separator and the main separator are thermally integrated. The column primarily separates the low boiling point and high boiling point material from the preliminary separator, and the top and bottom portions of the preliminary separator are respectively introduced into the feed stage of the main separator to separate the low, middle and high boiling point materials from the main separator. It is designed. On the other hand, in the case of the dividing wall distillation column 200, the dividing wall 201 is installed in the tower and the preliminary separator is integrated into the main separator.

The dividing wall distillation column 200 may have, for example, a structure as shown in FIG. 3. 3 shows an exemplary dividing wall distillation column 200. As shown in FIG. 3, the exemplary distillation column may have a structure in which an interior is divided by a partition wall 201 and includes an upper condenser 202, a lower reboiler 203, and the like. In addition, the interior of the dividing wall distillation column 200 is virtually divided by a dotted line in the drawing, for example, a top region 210 through which a low boiling point flow is discharged, a bottom region 220 through which a high boiling point flow is discharged, It may be divided into a raw material supply area 230 through which the feed is introduced and a product outlet area 240 through which the product flows out. The raw material supply area 230 may be an upper supply area 231 and a lower supply area 232. The product outlet region 240 may be divided into an upper product outlet region 241 and a lower product outlet region 242. As used herein, the term "upper and lower supply region" refers to the distillation column, that is, the space on the side where the feed is supplied, that is, the raw material supply region 230 of the space divided by the partition wall 201 in the structure of the dividing wall distillation column 200, respectively. When bisected in the longitudinal direction of may mean the upper and lower regions. In addition, the "upper and lower product outflow area" refers to the space on the side where the product flows out, that is, the product outflow area 240 in the space divided by the separation wall 201 inside the dividing wall distillation column 200, respectively. When bisected in the longitudinal direction of the distillation column, it may mean the upper and lower regions. Said "low boiling point flow" means a flow in which a relatively low boiling point component is rich among feed streams including three components of low boiling point, middle boiling point and high boiling point component, and said "high boiling point flow" means low boiling point and medium boiling point. A feed stream containing three components, a point and a high boiling point component, means a stream in which a relatively high boiling point component is rich.

In the purification method of the present application, the feed introduced into the raw material supply region 230 of the dividing wall distillation column 200 is purified in the dividing wall distillation column 200. In addition, a component having a relatively low boiling point in the feed introduced into the raw material supply region 230 moves toward the top region 210, and a component having a relatively high boiling point moves toward the bottom region 220. . The components having a relatively low boiling point among the components moved to the bottom region 220 are moved to the product outlet region 240 so as to flow out into the product flow or to the top region 210, and the bottom region ( The components having a relatively high boiling point among the components moved to 220 are discharged to the high boiling point flow in the bottom region 220. A portion of the high boiling point flow flowing out of the bottom region 220 is discharged into a flow of high boiling point component, and the other part is heated in the reboiler 203 and then re-introduced into the bottom region 220 of the dividing wall distillation column. Can be. Meanwhile, in the top region 210, a flow of low boiling point component having a very high moisture content flows out, and the flow flowing out of the top region 210 is condensed in the condenser 202, and a part of the condensed flow is discharged. The remaining part may be refluxed to the top region 210 of the dividing wall distillation column 200. In addition, the flow flowing back out of the column top region 210 is purified again in the dividing wall distillation column 200, thereby minimizing the amount of IPA flowing out of the column top region 210, and reducing the amount of water flowing out of the column top region 210. Can be maximized.

The specific kind of the dividing wall distillation column 200 that can be used in the purification method is not particularly limited. For example, a dividing wall distillation column having a general structure as shown in FIG. 3 may be used, or a distillation column designed to change the position or shape of the dividing wall in the distillation column in consideration of purification efficiency may be used. In addition, the number of stages and the inner diameter of the distillation column are not particularly limited, and for example, the number of stages derived from the distillation curve in consideration of the feed composition may be set.

In the dividing wall distillation column 200 which performs the purification process in the above method, for example, when a feed whose water content is adjusted to 500 ppm or less is introduced, the water content in the feed is 150 ppm or less, for example, through the purification process. It may be installed to be discharged down to 120 ppm or less, 110 ppm or less, 100 ppm or less, 80 ppm or less, 60 ppm or less, 50 ppm or less, 30 ppm or less or 10 ppm or less. Accordingly, in the refining step, water is removed from the feed fed to the dividing wall distillation column so that the water content of the feed is 150 ppm or less, for example, 120 ppm or less, 110 ppm or less, 100 ppm or less, 80 ppm or less, or 60 ppm or less. And 50 ppm or less, 30 ppm or less, or 10 ppm or less. Through the dividing wall distillation column 200, while controlling the water content in the above range can be purified IPA with high purity.

The dividing wall distillation column 200 may be installed such that, for example, a feed passing through the membrane system 100 is supplied to the raw material supply region 230 of the distillation column. Accordingly, in the refining process, a feed whose water content has passed through the dehydration process is adjusted to 500 ppm or less may be supplied to the raw material supply region 230 of the distillation column. When the feed is supplied to the dividing wall distillation column 200, in consideration of the composition of the feed, for example, as shown in FIG. 3, when the feed is supplied to the upper supply region 231, efficient purification may be possible.

Through this process, in the dividing wall distillation column 200, a product containing purified IPA and having a water content of 150 ppm or less is discharged from the lower product outlet region 242, preferably in the middle portion of the lower product outlet region 242. Can be installed as possible. That is, the purification method calculates a product containing purified IPA and having a water content of 150 ppm or less based on the bottom of the bottom product outlet region 242 of the dividing wall distillation column 200, preferably the top of the dividing wall distillation column 200. Obtained from 50 to 90%, 55% to 80%, or 60% to 75% of the theoretical stages. For example, when the theoretical stage of the dividing wall distillation column 200 is 100 stages, the product having a water content of 100 ppm or less may be discharged from 50 to 90 stages or 60 to 75 stages. The efficiency of the purification process can be further increased. In the above description, the "middle portion of the lower product outlet region" means a point where the lower product outlet region 242 is divided into two equal parts in the longitudinal direction of the dividing wall distillation column 200.

As described above, the theoretical stages of the dividing wall distillation column 200 necessary for controlling the moisture content of the feed having a water content of 500 ppm or less to 150 ppm or less are 70 to 120 stages, 80 stages to 110 stages, or 85 to 100 stages. However, the present invention is not limited thereto, and may be appropriately changed according to the flow rate and process conditions of the incoming feed.

On the other hand, in the case of the dividing wall distillation column 200, unlike the Petlyuk distillation column, if the design is determined, the flexibility of the operating conditions fluctuates due to the structural characteristics that cannot control the internal circulation flow rate. It is necessary to accurately control the disturbance and to determine the control structure that enables easy control. Further, in the dividing wall distillation column 200, the position of the feed end, the setting of the partition wall section, the position of the production point of the intermediate boiling point material, the total theoretical stage, The design structure and operation conditions of the distillation column, such as distillation temperature and distillation pressure, are very limited, and in particular, the design structure of the number of stages, feed stage and outlet of the distillation column according to the properties of the compound to be distilled. And operating conditions such as distillation temperature, pressure and reflux ratio should be changed specially. In the purification method of the present application, as described above, it is possible to provide operating conditions of the dividing wall distillation column 200 which is designed for the purification of the IPA to save energy and reduce the equipment cost.

In one example, as described above, a feed whose water content is adjusted to 500 ppm or less is introduced into the distillation wall distillation column 200, and the water content in the feed is 150 ppm or less through a purification process in the dividing wall distillation column 200. When adjusting, the reflux ratio of the column top region 210 of the dividing wall distillation column 200 may be adjusted in the range of 60 to 90, for example, 65 to 90, 70 to 85 or 75 to 85. For example, the higher the content of water in the feed introduced into the dividing wall distillation column 200, the more the reflux ratio of the top region 210 to remove the water in the feed and to obtain a high purity IPA need to be largely controlled, but the present application In the purification method of, the content of water in the feed introduced into the dividing wall distillation column 200 is adjusted to 500 ppm or less, and the reflux ratio of the top region 210 in the dividing wall distillation column 200 is adjusted to a specific range as described above. Thereby, the content of water in the IPA obtained in the bottom product outlet region 242 can be controlled very low.

For example, the feed may be supplied to the dividing wall distillation column 200 at a flow rate of about 5,000 Kg / hr to about 13,000 Kg / hr. In addition, the temperature of the feed is, for example, may be adjusted to about 50 ℃ to 135 ℃, 60 ℃ to 110 ℃ or 80 ℃ to 100 ℃ degree. By supplying the feed at the flow rate and temperature as described above it is possible to achieve an appropriate distillation efficiency.

As described above, the operation temperature of the top region 210 of the dividing wall distillation column 200 is 40 ° C. to 120 ° C. at the time of distillation which is performed by supplying a feed whose water content is adjusted to 500 ppm or less to the dividing wall distillation column 200. For example, it may be adjusted to about 45 ℃ to 110 ℃ or 50 ℃ to 100 ℃ degree. In this case, the operating pressure of the top region 210 of the dividing wall distillation column 200 is 0.1 Kg / cm ² to 10.0 Kg / cm ² , For example, 0.2 Kg / cm ² to 5.5 Kg / cm ² , 0.3 Kg / cm ² to 4.5 Kg / cm ² , 0.6 Kg / cm ² to 4.0 Kg / cm ² or 0.68 Kg / cm ² to 3.7 Kg / cm It can be adjusted to ^two degrees. At such operating temperatures and pressures, efficient distillation may be possible depending on the composition of the feed. In the present specification, the pressure means absolute pressure unless specifically defined otherwise.

Operation and pressure conditions inside the dividing wall distillation column 200 may be changed according to temperature and pressure conditions of the top region 210. In one example, when the temperature of the top region 210 of the dividing wall distillation column 200 is adjusted to 40 ℃ to 120 ℃, the outflow from the lower product outlet region 242 of the dividing wall distillation column 200 The temperature of the flow can be adjusted to between 60 ° C. and 130 ° C., for example, between 70 ° C. and 125 ° C., 75 ° C. and 120 ° C., or between 77.3 ° C. and 120 ° C. In addition, when the pressure of the top region 210 of the dividing wall distillation column 200 is adjusted to 0.2 Kg / cm ² to 5.5 Kg / cm ² , the lower product outlet region 242 of the dividing wall distillation column 200 The operating pressure is 0.3 Kg / cm ² to 6.0 Kg / cm ² , for example 0.5 Kg / cm ² to 5.0 Kg / cm ² , 0.8 Kg / cm ² to 4.0 Kg / cm ² or 0.843 Kg / cm ² to It can be adjusted to about 3.86 Kg / cm ² . At such operating temperatures and pressures, efficient distillation may be possible depending on the composition of the feed.

In addition, when the temperature of the top region 210 of the dividing wall distillation column 200 is adjusted to 40 ℃ to 120 ℃, the operating temperature of the top bottom region 220 of the dividing wall distillation column 200, 80 ℃ to 160 ℃, for example, it can be adjusted to about 90 ℃ to 160 ℃, 95 ℃ to 158 ℃ or 104 ℃ to 156 ℃ degree. In addition, when the pressure of the top region 210 of the dividing wall distillation column 200 is adjusted to 0.2 Kg / cm ² to 5.5 Kg / cm ² , the operating pressure of the top region 220 of the dividing wall distillation column 200. Silver, 0.3 Kg / cm ² to 6.0 Kg / cm ² , for example 0.8 Kg / cm ² to 5.0 Kg / cm ² , 0.9 Kg / cm ² to 4.0 Kg / cm ² or 0.91 Kg / cm ² to 3.93 Kg / cm ² can be adjusted. At such operating temperatures and pressures, efficient distillation may be possible depending on the composition of the feed.

In the above, the operating conditions of the dividing wall distillation column 200 may be further adjusted as necessary in consideration of purification efficiency and the like.

Other conditions of the dividing wall distillation column 200 in which the purification process is performed, for example, the number of stages or the inner diameter of each distillation column are not particularly limited. For example, the theoretical number of stages of the dividing wall distillation column 200 may be determined based on the theoretical number calculated by the distillation curve of the feed. In addition, the flow rate of the upper and lower discharges in the dividing wall distillation column 200, for example, may be set to achieve the above-described operating pressure and temperature.

The present application also relates to a purification apparatus of IPA. An exemplary purification apparatus may be an apparatus for application to the purification method described above.

Accordingly, the purification apparatus, for example, when the feed described above is supplied, the dehydration means (D) and the feed through the dewatering means (D) installed to discharge the water content of the feed to 500 ppm or less is discharged It may include a purifying means (P) which can be introduced to proceed with the purification process.

Specific details related to the refining apparatus may be applied, for example, to the same or similar items.

For example, the dewatering means D may be the membrane system 100 and the

columns

110, 111 filled with the adsorbent.

As the membrane system 100 of the dehydration means (D), any system using a separation membrane is not particularly limited. For example, a pervaporation system or a vapor permeation system may be used. have.

As described above, the separator that may be used in the pervaporation system or the vapor permeation system may be an organic separator such as a polymer membrane, an inorganic separator, an organic-inorganic separator prepared by mixing an organic material and an inorganic material, etc. according to the type of material used. In the dehydration means (D) of the present application, various separators known in the art may be variously used according to a desired separation component. For example, as the hydrophilic separator, a separator made of silica gel, a separator made of a polymer such as PVA or polyimide, and a zeolite separator may be used, but may be appropriately changed in consideration of the desired dehydration amount and the composition of the feed. For example, a zeolite membrane of Pervatech, a zeolite A membrane of i3nanotec, a zeolite NaA membrane, etc. may be used as the zeolite separator, but is not limited thereto. In order to maintain the strength of the separator, the polymer separator may be coated with an inorganic material.

In one example, the adsorbent filled in the columns (110, 111) may include a molecular sieve, silica gel, activated alumina, activated carbon or ion exchange resin.

In one example, the dehydration means (D) may include two or

more columns

110 and 111 in which molecular sieves are filled.

The refining apparatus may include, for example, refining means P through which a feed having passed through the dehydration means D may be introduced to perform a refining process, and the refining means P is a dividing wall distillation column. Wall Column, DWC).

In the above-described dividing wall distillation column 200, for example, the feed passing through the dehydration means (D) is to be supplied to the raw material supply region 230, for example, the upper supply region 231 of the dividing wall distillation column (200). It may be installed. In addition, the dividing wall distillation column 200 may be installed such that the product including the IPA is discharged from the middle portion of the lower product outlet region 242, preferably the lower product outlet region 242.

Detailed description related to the dividing wall distillation column 200 is the same as described in the above-described purification method, it will be omitted.

In this application, IPA can be obtained in high purity from a feed comprising water and IPA with minimal energy consumption.

1 exemplarily shows the progress of the method.

2 shows an example of the dehydration means used in the method.

3 is a view illustratively showing purification means used in the method.

4 is a view showing an exemplary purification device according to a first embodiment of the present application.

5 and 6 are views exemplarily showing a purification apparatus according to a comparative example of the present application.

The method is described in detail below through examples and comparative examples, but the scope of the method and apparatus is not limited to the examples given below.

실시예 1Example 1

As shown in FIG. 4, IPA was purified using a dehydration means and a dividing wall column connected to the dehydration means. Specifically, the dehydration means used a device in which a membrane system and a column filled with molecular sieves are sequentially connected, and the membrane system uses a permeation evaporation system including a membrane (HybSi membrane, Pervatech) device and a vacuum device. As the molecular sieve, zeolite 3A having an effective pore average size of about 3 microns was used, and two columns having a packed volume of about 3 m ³ were used. Regeneration of the molecular sieve was carried out using a means capable of supplying nitrogen gas at a flow rate of about 1,314 Nm ³ / hr at about 230 ℃. As a feed, a liquid feed containing 98.6 wt% IPA, about 3,000 ppm water, and about 1.1 wt% other impurities was used. The feed is supplied to the dehydration means at a temperature of 90 ° C. to adjust the water content in the feed passing through the pervaporation system to about 1,000 ppm, and the dewatering process so that the water content in the feed passing through the column is about 300 ppm. Proceeded. Subsequently, a feed having a water content of about 300 ppm after the dehydration process is introduced into a raw material supply region of the dividing wall distillation column, specifically, 20 stages of the dividing wall distillation column having 90 theoretical stages, and the purification is performed. Silver bottom product effluent zone, specifically 60 stages of dividing wall column with 90 theoretical stages.

In the above, the reflux ratio of the column top region of the dividing wall distillation column was adjusted to 80, and the operating temperature and the pressure of the column top region were adjusted to about 63 ° C. and 1.12 Kg / cm ² , respectively. In this case, the operating temperature and pressure of the bottom product outlet region where the high purity IPA flows out were about 100 ° C. and 1.33 Kg / cm ² , respectively, and the operating temperature and pressure of the bottom area were about 117 ° C. and 1.37 Kg / cm ^{2, respectively} . .

In this case, the content of the high boiling point component in the IPA obtained in the lower product outflow region was measured to be about 42 ppm.

실시예 2Example 2

Purification was carried out in the same manner as in Example 1 except that the reflux ratio of the column top region was adjusted to 85.

실시예 3Example 3

The purification was carried out in the same manner as in Example 1 except that the reflux ratio of the column top region was adjusted to 76.

실시예 4Example 4

Purification was carried out in the same manner as in Example 1 except that the product containing IPA was obtained in 40 stages of a 90-stage dividing wall distillation column.

실시예 5Example 5

Purification was carried out in the same manner as in Example 1 except that the product containing IPA was obtained in 70 stages of a distillation column having a theoretical stage of 90 stages.

In this case, the content of the high boiling point component in the IPA obtained in the lower product outflow region was measured to be about 52 ppm.

실시예 6Example 6

The process was carried out in the same manner as in Example 1 except that the water content in the feed introduced through the dehydration means to the purification means was adjusted to about 500 ppm. In this case, the reflux ratio of the top section of the dividing wall distillation column was adjusted to 85, and the operating temperature and pressure were adjusted to about 65 ° C. and 1.12 Kg / cm ² , respectively, and the operating temperature and pressure of the column bottom section were about 117 ° C. and 1.35, respectively. Kg / cm ² was adjusted.

실시예 7 Example 7

Purification was carried out in the same manner as in Example 1 except that the operating temperature and the pressure in the top region were adjusted to about 50 ° C. and 0.68 Kg / cm ² , respectively.

In this case, the operating temperature and pressure in the bottom product outlet region were about 77.3 ° C. and 0.843 Kg / cm ² , respectively, and the operating temperature and pressure in the bottom region were about 104 ° C. and 0.91 Kg / cm ² , respectively.

실시예 8 Example 8

Purification was carried out in the same manner as in Example 1 except that the operating temperature and the pressure in the top region were adjusted to about 100 ° C. and 3.7 Kg / cm ² , respectively.

In this case, the operating temperature and pressure in the bottom product outlet region were about 120 ° C. and 3.86 Kg / cm ² , respectively, and the operating temperature and pressure in the bottom region were about 156 ° C. and 3.93 Kg / cm ² , respectively.

비교예 1Comparative Example 1

A liquid feed containing 98.6% by weight of IPA, about 3,000 ppm of water, and about 1.1% by weight of other impurities was purified by flowing into a purification apparatus connected to two general distillation columns without undergoing a dehydration process as shown in FIG. 5. In this case, the tower operation temperature and pressure of the first distillation column were adjusted to about 76 ° C. and 1.12 Kg / cm ² , respectively, and the tower operation temperature and pressure were adjusted to about 93 ° C. and 1.54 Kg / cm ² . In addition, the top operating temperature and pressure of the second distillation column were adjusted to about 83 ° C. and 1.04 Kg / cm ² , respectively, and the lower operating temperature and pressure were adjusted to about 110 ° C. and 1.18 Kg / cm ² .

비교예 2Comparative Example 2

The process was carried out in the same manner as in Example 1 except that the feed permeated through the membrane system was introduced into a purification apparatus connected to two general distillation columns instead of the dividing wall distillation column. In this case, the top operating temperature and pressure of the first distillation column were adjusted to about 63 ° C. and 1.12 Kg / cm ² , respectively, and the bottom operating temperature and pressure were adjusted to about 93 ° C. and 1.54 Kg / cm ² . In addition, the top operating temperature and pressure of the second distillation column were adjusted to about 83 ° C. and 1.04 Kg / cm ² , respectively, and the bottom operating temperature and pressure were adjusted to about 110 ° C. and 1.18 Kg / cm ² .

비교예 3Comparative Example 3

Same as Example 1 except that a liquid feed comprising 98.6% by weight of IPA, about 3,000 ppm of water and about 1.1% by weight of other impurities was introduced directly into the dividing wall distillation column as shown in FIG. 3 without undergoing a dehydration process. The process was carried out in a manner. In this case, the reflux ratio of the top section of the dividing wall distillation column was adjusted to 52, and the operating temperature and pressure of the top section were adjusted to about 76 ° C. and 1.12 Kg / cm ² , respectively. And controlled at 1.37 Kg / cm ² .

비교예 4Comparative Example 4

Purification was carried out in the same manner as in Example 1 except that the product containing IPA was obtained in 35 stages of a 90-stage dividing wall distillation column.

비교예 5 Comparative Example 5

Purification was carried out in the same manner as in Example 1 except that the product containing IPA was obtained in 85 stages of the distillation column having a theoretical stage of 90 stages.

In this case, the content of the high boiling point component in the IPA obtained in the lower product outflow zone was measured to be about 590 ppm.

비교예 6Comparative Example 6

The process was carried out in the same manner as in Example 1 except that the water content in the feed introduced through the dehydration means to the purification means was adjusted to about 700 ppm.

The total energy usage and water content in the IPA used in the above Examples and Comparative Examples are summarized in Table 1 and Table 2 below.

Table 1

		Example 1	Example 2	Example 3	Example 4	Example 5	Example 6	Example 7	Example 8
HEAT DUTY (Gcal / hr)	Condenser	1.49	1.6	1.43	1.49	1.49	1.78	1.43	1.59
HEAT DUTY (Gcal / hr)	Scraping	1.47	1.58	1.41	1.47	1.47	1.76	1.37	1.74
Energy savings (Gcal / hr)		1.55	1.44	1.61	1.55	1.55	1.26	1.65	1.28
Energy saving rate (%)		51%	48%	53%	51%	51%	42%	55%	42%
Moisture Content in IPA (ppm)		89	100	110	110	100	100	89	100
Energy savings: Energy savings compared to Comparative Example 1, Energy savings: Energy savings compared to Comparative Example 1

TABLE 2

		Comparative Example 1	Comparative Example 2	Comparative Example 3	Comparative Example 4	Comparative Example 5	Comparative Example 6
HEAT DUTY (Gcal / hr)	Condenser	3.13	2.5	2.02	1.49	1.49	3.10
HEAT DUTY (Gcal / hr)	Scraping	3.02	2.4	2	1.47	1.47	2.99
Energy savings (Gcal / hr)		0	0.62	1.02	1.55	1.55	0.03
Energy saving rate (%)		0%	21%	34%	51%	51%	One%
Moisture Content in IPA (ppm)		100	100	100	130	100	100
Energy savings: Energy savings compared to Comparative Example 1, Energy savings: Energy savings compared to Comparative Example 1

Claims

Supplying a feed comprising isopropyl alcohol and water to dewatering means comprising a column packed with a membrane system and an adsorbent to remove water; And

Purifying the isopropyl alcohol comprising the step of removing water from the dehydration means and supplying a feed having a controlled water content to a dividing wall distillation column.
The method of claim 1, wherein the membrane system is a pervaporation system or a vapor permeation system.
The method for purifying isopropyl alcohol according to claim 1, wherein the adsorbent comprises molecular sieve, silica gel, activated alumina, activated carbon or ion exchange resin.
The method of claim 1, wherein the step of removing water comprises supplying a feed having a water content of 1,200 ppm to 5,000 ppm to the dewatering means, and adjusting the water content of the feed in the dewatering means to 500 ppm or less. Purification method.
The method of claim 1 wherein the step of removing water comprises supplying a feed having a water content of 1,200 ppm to 5,000 ppm to the membrane system to adjust the water content to 500 ppm to 1,200 ppm and the water content to 500 ppm to 1,200 ppm. A method for purifying isopropyl alcohol comprising feeding a feed to a column packed with an adsorbent to adjust the water content to 50 ppm to 500 ppm.
The method of claim 1, wherein the step of purifying includes removing water from the dehydration means and supplying a feed having a water content of 500 ppm or less to a dividing wall distillation column, so that the water content is controlled to 150 ppm or less. Method for Purifying Isopropyl Alcohol.
The distillation wall type distillation column according to claim 1, wherein the dividing wall distillation column is divided into a raw material supply region, a top region, a bottom region and a product outlet region, and the product outlet region is divided into an upper product outlet region and a lower product outlet region.

The step of purifying removes water from the dehydration means to supply a feed whose water content is adjusted to 500 ppm or less to the raw material supply region of the dividing wall distillation column, and performs purification in the dividing wall distillation column, and purifies the purified iso A process for purifying isopropyl alcohol comprising obtaining effluent containing propyl alcohol and having a water content of 150 ppm or less in the bottom product outlet of the dividing wall distillation column.
8. The process according to claim 7, wherein the effluent comprising purified isopropyl alcohol and having a water content of 150 ppm or less is obtained at a stage of 50% to 90% of theoretical stage calculated on the top of the dividing wall distillation column.
The method for purifying isopropyl alcohol according to claim 7, comprising adjusting the temperature of the column top region of the dividing wall distillation column to 40 ° C to 120 ° C.
8. The method for purifying isopropyl alcohol according to claim 7, comprising adjusting the pressure of the top region of the dividing wall distillation column to 0.1 to 10.0 Kg / cm 2 .
10. The process for purifying isopropyl alcohol according to claim 9, wherein the temperature of the stream flowing out of the bottom product region of the dividing wall distillation column is from 60 deg.
The process for purifying isopropyl alcohol according to claim 10, wherein the pressure of the bottom product outlet region of the dividing wall distillation column is 0.3 to 6.0 Kg / cm 2 .
The method for purifying isopropyl alcohol according to claim 9, wherein the temperature of the bottom region of the dividing wall distillation column is 80 ° C to 160 ° C.
The method for purifying isopropyl alcohol according to claim 10, wherein the pressure in the bottom region of the dividing wall distillation column is 0.3 to 6.0 Kg / cm 2 .
Dewatering means comprising a membrane system and a column packed with an adsorbent, wherein a feed comprising isopropyl alcohol and water is supplied and regulates and discharges the water content of the feed; And

Apparatus for purifying isopropyl alcohol comprising a dividing wall distillation column in which a feed having passed through the dehydration means is introduced to undergo a purification process.
The purification apparatus of isopropyl alcohol according to claim 15, wherein the membrane system is a pervaporation system or a vapor permeation system.
16. The apparatus for purifying isopropyl alcohol according to claim 15, wherein the adsorbent comprises molecular sieve, silica gel, activated alumina, activated carbon or ion exchange resin.
18. The apparatus of claim 17, wherein the molecular sieve comprises zeolite, silica-alumina or silicate alumina.
17. The dividing wall distillation column according to claim 15, wherein the dividing wall distillation column is divided into a raw material supply zone, a column top region, a bottom bottom region, and a product outlet region, and the product outlet region is divided into an upper product outlet region and a lower product outlet region.

A feed whose water content is adjusted to 500 ppm or less by dewatering means is fed to the raw material supply zone of the dividing wall distillation column, and the discharge containing purified isopropyl alcohol and having a water content of 150 ppm or less is obtained from the distillation column distillation column. Purification apparatus exiting the bottom product outlet area.