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WO2025115671A1 - Procédé et dispositif de production d'alcool isopropylique purifié - Google Patents

Procédé et dispositif de production d'alcool isopropylique purifié Download PDF

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Publication number
WO2025115671A1
WO2025115671A1 PCT/JP2024/040792 JP2024040792W WO2025115671A1 WO 2025115671 A1 WO2025115671 A1 WO 2025115671A1 JP 2024040792 W JP2024040792 W JP 2024040792W WO 2025115671 A1 WO2025115671 A1 WO 2025115671A1
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WIPO (PCT)
Prior art keywords
phase separation
isopropyl alcohol
phase liquid
phase
azeotropic
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Pending
Application number
PCT/JP2024/040792
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English (en)
Japanese (ja)
Inventor
貴史 徳永
義晶 山下
俊輔 保坂
衛 清松
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Tokuyama Corp
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Tokuyama Corp
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Priority to JP2025512053A priority Critical patent/JP7695493B1/ja
Publication of WO2025115671A1 publication Critical patent/WO2025115671A1/fr
Pending legal-status Critical Current
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0208—Separation of non-miscible liquids by sedimentation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36—Azeotropic distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/02—Monohydroxylic acyclic alcohols
    • C07C31/10—Monohydroxylic acyclic alcohols containing three carbon atoms

Definitions

  • the present invention relates to a method and apparatus for producing purified isopropyl alcohol by dehydrating crude isopropyl alcohol that contains water as an impurity.
  • IPA Isopropyl alcohol
  • IPA has the ability to dissolve both water and organic solvents, and is widely used as a paint solvent, ink solvent, and various synthetic raw materials. Furthermore, high-purity IPA is used in large quantities in the rinsing section of semiconductor substrates in semiconductor manufacturing equipment, and its usage is expected to continue to increase in the future.
  • the direct hydration of propylene is one example of a method for synthesizing IPA.
  • the crude IPA product synthesized in this way is usually purified by distillation, but in order to obtain high-purity IPA, it is necessary to combine multiple distillation steps.
  • a method that is known to have a high purification effect is to carry out a low-boiling distillation step in which low-boiling impurities with a boiling point lower than IPA are removed from the top of the distillation tower, and then a high-boiling distillation step in which high-boiling impurities with a boiling point higher than IPA are removed from the bottom of the distillation tower.
  • an azeotropic distillation step is carried out in which an azeotropic agent such as benzene is mixed and azeotropic distillation is performed (see, for example, Patent Document 1).
  • IPA waste liquid recovered from semiconductor manufacturing equipment is generally burned, but this process releases carbon dioxide, which is believed to be a cause of global warming. Therefore, from the perspective of environmental conservation, it has been desirable to reduce the amount of IPA waste liquid disposed of.
  • the inventors have continued to conduct intensive research in light of the above problems. As a result, they have discovered that the above problems can be solved by azeotropic distillation of an upper phase liquid containing an azeotropic agent, water, and isopropyl alcohol obtained by phase separation in the presence of an azeotropic agent, rather than directly azeotropically distilling crude IPA containing water as an impurity, and have thus completed the present invention.
  • one aspect of the present invention is a method for producing purified isopropyl alcohol by dehydrating crude isopropyl alcohol containing water as an impurity, which includes a phase separation step in which a mixture of the crude isopropyl alcohol and an azeotropic agent is placed in a phase separation tank and phase-separated into an upper phase liquid containing the azeotropic agent, water, and isopropyl alcohol, and a lower phase liquid containing water, and an azeotropic distillation step in which the upper phase liquid is azeotropically distilled in an azeotropic distillation tower to extract a distillate containing an azeotropic mixture of the azeotropic agent and water, and a bottoms liquid containing isopropyl alcohol, and the distillate is supplied to the phase separation tank.
  • Another aspect of the present invention is an apparatus for producing purified isopropyl alcohol by dehydrating crude isopropyl alcohol containing water as an impurity, the apparatus comprising: a phase separation tank for containing a mixture of the crude isopropyl alcohol and an azeotropic agent and for separating the mixture into an upper phase liquid containing the azeotropic agent, water, and isopropyl alcohol, and a lower phase liquid containing water; and an azeotropic distillation tower for azeotropically distilling the upper phase liquid.
  • the phase separation tank is provided with a first supply pipe for supplying the crude isopropyl alcohol to the phase separation tank, and a second supply pipe for supplying the upper phase liquid to the phase separation tank.
  • a second supply pipe is connected to the raw material supply stage of the tower, a third supply pipe is connected to the top of the azeotropic distillation tower to supply a distillate containing an azeotropic mixture of the entrainer and water to the phase separation tank, a withdrawal pipe is connected to the bottom of the azeotropic distillation tower to withdraw a bottom product containing isopropyl alcohol, and a fourth supply pipe is connected to any one of the first supply pipe, the phase separation tank, the second supply pipe, the azeotropic distillation tower, and the third supply pipe to supply the entrainer.
  • This is an apparatus for producing purified isopropyl alcohol.
  • purified IPA can be efficiently produced from crude IPA that contains water as an impurity, using a small amount of heat.
  • FIG. 1 is a schematic diagram showing a purified IPA production apparatus according to one embodiment of the present invention.
  • FIG. 2 is a cross-sectional view showing the outline of the structure of the phase separation tank of FIG. 1.
  • the crude IPA is not particularly limited as long as it contains water as an impurity, and examples thereof include a crude IPA product obtained by a synthesis method such as a direct hydration method of propylene, and an IPA waste liquid recovered from various industrial facilities.
  • an IPA waste liquid recovered from a semiconductor substrate manufacturing apparatus is preferable.
  • an IPA waste liquid recovered from a developing section or a pre-wet section of a semiconductor substrate manufacturing apparatus corresponds to the IPA waste liquid.
  • a semiconductor substrate manufacturing apparatus is provided with a rinsing section that removes moisture adhering to the surface of the substrate after a cleaning section that cleans the substrate with an aqueous cleaning agent, and a large amount of IPA is used as a rinsing liquid.
  • an IPA waste liquid recovered from a rinsing section is also preferably applied.
  • the crude IPA product and IPA waste liquid can be used as the crude IPA, it is preferable to use the water-containing IPA obtained by refining the crude IPA product and IPA waste liquid as the crude IPA.
  • the water content of the crude IPA is usually 1% by mass or more and 50% by mass or less, more preferably 10% by mass or more and 20% by mass or less.
  • Distillation is a suitable method for purifying the IPA crude product and IPA waste liquid.
  • An example of distillation is a method for removing high boiling impurities from the bottom of a high boiling distillation tower. It is preferable to apply the distillate containing an azeotropic mixture of IPA and water (IPA 88% by mass, water 12% by mass) extracted from the top of the high boiling distillation tower to the crude IPA. Note that, before distillation in the high boiling distillation tower, low boiling impurities may usually be removed from the top of the low boiling distillation tower.
  • the upper phase liquid obtained by phase separation of the mixture of crude IPA and the azeotropic agent is azeotropically distilled. That is, azeotropic distillation is a distillation in which an azeotropic agent is added to separate a mixture of liquids that are difficult or impossible to separate by normal distillation, and an azeotropic mixture is generated and separated.
  • the azeotropic agent is used to remove water from the upper phase liquid.
  • the azeotropic agent a compound that has a lower boiling point than IPA and forms an azeotropic mixture with water is used.
  • azeotropic agent a compound that forms an upper phase containing the azeotropic agent, water, and IPA and a lower phase containing water when the mixture of crude IPA and the azeotropic agent is phase separated is used.
  • the azeotropic agent include benzene, toluene, cyclohexane, and isopropyl ether. Among these, benzene is particularly preferable.
  • the amount of azeotropic agent added is preferably 50 parts by mass or more and 1,000 parts by mass or less, and more preferably 80 parts by mass or more and 500 parts by mass or less, per 100 parts by mass of crude IPA.
  • the crude IPA is accommodated in a phase separation tank in a state where the azeotropic agent is mixed therein before azeotropic distillation. Then, the upper phase liquid formed in the phase separation tank, which contains the azeotropic agent, water, and IPA, is separated and azeotropically distilled.
  • the crude IPA is directly azeotropically distilled (see, for example, Patent Document 2).
  • Patent Document 2 Japanese Patent Document 2
  • a large amount of crude IPA is azeotropically distilled, not only the amount of heat is increased, but also the diameter of the azeotropic distillation tower is increased, making it impossible to efficiently produce purified IPA.
  • the crude IPA is not directly supplied to the azeotropic distillation tower, but is contained in the phase separation tank in a state where the azeotropic agent is mixed therewith.
  • the crude IPA is separated into an upper phase liquid containing the azeotropic agent, water, and IPA, and a lower phase liquid containing water. Therefore, by separating the upper phase liquid and supplying it to the azeotropic distillation tower, the total amount and water content of the upper phase liquid to be azeotropically distilled can be reduced relative to the crude IPA, and as a result, the amount of heat consumed during azeotropic distillation can be reduced.
  • the water content of the upper phase liquid obtained from crude IPA with a water content of 12% by mass can be reduced to 0.1% by mass or more and 10% by mass or less, more preferably 0.5% by mass or more and 4% by mass or less.
  • phase separation tank In FIG. 1, the first supply pipe 1 for supplying the crude IPA, which is the liquid to be treated, is connected to the phase separation tank 4, not to the azeotropic distillation tower 2. As a result, the crude IPA is temporarily accommodated inside the phase separation tank 4. At this time, the crude IPA is supplied so that the crude IPA and the azeotropic agent are mixed and accommodated in the phase separation tank 4, as will be described later. As a result, in the phase separation tank 4, phase separation occurs into an upper phase liquid 5 containing the azeotropic agent, water, and IPA, and a lower phase liquid 6 containing water. In this embodiment, the upper phase liquid 5 formed by phase separation is supplied to the raw material supply stage of the azeotropic distillation tower 2 via the second supply pipe 7, and azeotropic distillation is performed.
  • the phase separation tank 4 is not particularly limited as long as it is capable of separating the liquid into an upper phase liquid 5 and a lower phase liquid 6 due to the difference in specific gravity, and may be appropriately selected from known decanters, settlers, etc.
  • the phase separation tank 4 preferably has a structure shown in FIG. 2.
  • the phase separation tank 4 has the following features: a) a phase separation chamber 8 in which a mixture of crude IPA and an azeotropic agent is accommodated and separated into an upper phase liquid 5 and a lower phase liquid 6; b) an upper phase liquid storage chamber 10 adjacent to the phase separation chamber 8 via a first partition wall 9a on one side of the phase separation chamber 8, and in which the upper phase liquid 5 that overflows the first partition wall 9a and flows in from the phase separation chamber 8 is stored; c) a lower phase liquid storage chamber 11 adjacent to the phase separation chamber 8 via a second partition wall 9b on the other side of the phase separation chamber 8 and storing the lower phase liquid 6 sent from the phase separation chamber 8 via a liquid sending pipe 14;
  • the separation property of the upper phase liquid 5 can be further improved, which is preferable.
  • the second supply pipe 7 is connected to the lower end region of the upper phase liquid storage chamber 10.
  • the liquid supply pipe 14 is a communicating pipe whose first opening end is connected to the lower phase liquid 6 contained in the phase separation chamber 8 and whose second opening end is connected to the lower phase liquid storage chamber 11.
  • the communicating pipe has an upward bent portion 12 including the second opening end, the highest part of which is at a height corresponding to the upper end region of the first partition wall 9a, and a branch portion 13 branching off from the upward bent portion 12, whose third opening end is connected to the gas phase part of the phase separation tank 4 at a position higher than the upper end of the first partition wall 9a.
  • the height of the upward bent portion 12 corresponds to the height of the upper end region of the first partition wall 9a, so that the inflow amount of the upper phase liquid 5 and the delivery amount of the lower phase liquid 6 are well balanced.
  • the height of the upward bent portion 12 may be such that the balance between the inflow amount of the upper phase liquid 5 and the delivery amount of the lower phase liquid 6 is well maintained, and the capacity of the phase separation chamber 8 and the lower phase liquid storage chamber 11 are each maintained at the desired amount.
  • the height of the upward bent portion 12 is usually 1/9, preferably 1/10 of the distance from the upper end of the first partition wall 9a to the lower end of the first partition wall 9a in the downward direction.
  • the pressure of the gas phase section of the phase separation tank 4 to which the third opening end is connected is not particularly limited, but from the viewpoint of preventing the inclusion of air and the separation property in distillation, it is preferably 900 hPa or more and 4013 hPa or less, and more preferably 1013 hPa or more and 2013 hPa or less.
  • the third opening end is connected to the gas phase of the phase separation tank 4 as shown in FIG. 2.
  • the third opening end is located at a position at least 40 cm higher than the upper end of the first partition wall 9a, and preferably at a position at least 50 cm higher.
  • the third opening end may also be connected to the outside of the phase separation tank 4.
  • phase separation chamber 8 From the viewpoint of stably separating the upper phase liquid 5 and the lower phase liquid 6, it is preferable to maintain a state in which the lower phase liquid 6 is held at a constant height in the phase separation chamber 8. For this reason, it is preferable to previously store a constant amount of water in the phase separation chamber 8, specifically, an amount of water that allows the residence time of the mixture of crude IPA and azeotropic agent in the phase separation chamber 8 to be 10 minutes or more and 90 minutes or less.
  • the amount of water previously stored in the phase separation chamber 8 is generally an amount equivalent to a height of 50 cm or more and 300 cm or less from the bottom of the phase separation chamber 8.
  • the flow rate of the crude IPA is preferably 0.1 m/s or more and 2 m/s or less, more preferably 0.3 m/s or more and 1 m/s or less.
  • the mixture of crude IPA and azeotropic agent is phase-separated before azeotropic distillation, so a significantly larger amount of the mixture is supplied to the phase separation tank 4 than when the mixture is phase-separated after azeotropic distillation.
  • using a phase separation tank 4 having the structure shown in Figure 2 is particularly effective because it has excellent separability between the upper phase liquid 5 and the lower phase liquid 6 and can minimize contamination with components of other phases.
  • the upper phase liquid 5 is supplied to the raw material supply stage of the azeotropic distillation column 2 from the upper phase liquid storage chamber 10 via the second supply pipe 7. Then, a first distillate containing an azeotropic mixture of an entrainer and water and IPA, which is extracted from the top of the azeotropic distillation column 2 via the condenser 3, is supplied to the phase separation tank 4 via the third supply pipe 15. On the other hand, a first bottoms containing IPA is extracted from the bottom of the azeotropic distillation column 2 via the first extraction pipe 16. At this time, the first bottoms may be used as purified IPA, or, as described below, the first bottoms may be purified and used as purified IPA.
  • the first distillate has an entrainer content of 40% by mass or more and 80% by mass or less, a water content of 1% by mass or more and 10% by mass or less, and an IPA content of 14% by mass or more and 54% by mass or less. It is even more preferable that the first distillate has an entrainer content of 40% by mass or more and 50% by mass or less, a water content of 2% by mass or more and 8% by mass or less, and an IPA content of 40% by mass or more and 50% by mass or less.
  • the azeotropic distillation tower 2 may be either a plate tower or a packed tower, but is preferably a plate tower.
  • the theoretical number of plates in the azeotropic distillation tower 2 is preferably 10 to 200, more preferably 20 to 50.
  • Examples of the plates in a plate tower include cross-flow trays and shower trays.
  • Examples of the packing in a packed tower include Raschig rings and Lessing rings.
  • Examples of the materials for the tower and packing include iron, stainless steel, Hastelloy, borosilicate glass, quartz glass, and fluororesin (e.g., polytetrafluoroethylene).
  • the upper phase liquid 5, which has a reduced water content compared to crude IPA, is azeotropically distilled, so the amount of heat consumed can be significantly reduced. This allows the azeotropic distillation tower 2 to be made smaller than when crude IPA is azeotropically distilled.
  • the number of theoretical stages of the feed stage of the azeotropic distillation tower 2 to the bottom of the tower is usually 5 or more, and more preferably 10 to 30. It is preferable to confirm the total theoretical number of stages of the azeotropic distillation tower 2 by actually operating it and performing a composition analysis.
  • the gauge pressure at the top of the azeotropic distillation tower 2 is not particularly limited, but is, for example, 0.0 MPaG or more and 0.1 MPaG or less. In this case, the temperatures at the top and bottom of the azeotropic distillation tower 2 may be set appropriately according to the gauge pressure.
  • the water content of the first bottoms varies depending on the type of azeotropic agent used, but is usually 1% by mass or less, and preferably 1000 ppm to 1 ppm.
  • the purity of the first bottoms (excluding the water content) is usually 99.9% by mass or more, and preferably 99.99% by mass or more to 99.999999% by mass or less.
  • the first distillate is supplied to the phase separation tank 4 via the third supply pipe 15 and circulated. That is, the entrainer, water, and IPA contained in the first distillate are phase-separated again into an upper phase liquid 5 and a lower phase liquid 6, and the upper phase liquid 5 is azeotropically distilled, thereby increasing the recovery rate of IPA.
  • a third supply pipe 15 is provided in parallel with the first supply pipe 1, but the third supply pipe 15 may also be connected to the first supply pipe 1.
  • a fourth supply pipe 17 is provided to supply an azeotropic agent to the phase separation tank 4, but the fourth supply pipe 17 may be connected to any of the first supply pipe 1, the second supply pipe 7, the azeotropic distillation tower 2, and the third supply pipe 15.
  • the lower phase liquid 6 contains water and IPA. Specifically, the content of IPA in the lower phase liquid 6 is 5% by mass or more and 50% by mass or less, preferably 10% by mass or more and 30% by mass or less. For this reason, the lower phase liquid 6 is supplied to the raw material supply stage of the IPA recovery distillation column 19 via the fifth supply pipe 18, and a side cut liquid containing an azeotropic mixture of IPA and water is extracted from the upper side of the IPA recovery distillation column 19. Then, the side cut liquid is supplied to the phase separation tank 4 via the sixth supply pipe 20 and circulated.
  • the water and IPA contained in the side cut liquid are phase-separated again into the upper phase liquid 5 and the lower phase liquid 6, and the upper phase liquid 5 is azeotropically distilled, so that the recovery rate of IPA is increased.
  • the lower phase liquid 6 may be disposed of without being distilled.
  • the second distillate may also be extracted from the top of the column.
  • a second bottoms liquid containing water is extracted from the bottom of the IPA recovery distillation column 19 via a second extraction pipe 21.
  • distillation can be performed under conditions that conform to the distillation conditions in the azeotropic distillation column 2, allowing the second distillate containing an azeotropic mixture of IPA and water to be efficiently extracted from the top or upper side of the column.
  • IPA waste liquid recovered from the rinsing section of a semiconductor substrate manufacturing device may contain low-boiling impurities such as methanol and ethanol.
  • a third distillate containing low-boiling impurities is extracted from the top of the IPA recovery distillation column 19 via the third extraction pipe 22.
  • the third distillate may be disposed of.
  • the first bottoms may be purified by adsorption or the like.
  • the first bottoms may also be purified by filtration to remove metal particles, inorganic particles, organic particles, etc.
  • the first bottoms may be purified by an ion exchange resin or the like to remove metal ions, etc.
  • Example 1 A crude IPA derived from an aqueous IPA waste liquid recovered from a semiconductor manufacturing apparatus equipped with a semiconductor substrate rinsing section was purified by an apparatus obtained by partially modifying the purified IPA manufacturing apparatus shown in Figures 1 and 2 to obtain a purified IPA.
  • the crude IPA used was an azeotropic mixture (IPA 88% by mass, water 12% by mass) obtained by subjecting the IPA waste liquid to low-boiling distillation for removing low-boiling impurities from the top of the tower and then high-boiling distillation for removing high-boiling impurities from the bottom of the tower.
  • the capacity of the phase separation chamber 8 was 24 L
  • the capacity of the upper phase liquid storage chamber 10 was 15 L
  • the capacity of the lower phase liquid storage chamber 11 was 15 L
  • the height of the upper end of the first partition wall 9a was 30 cm lower than the height of the second partition wall 9b, and was spaced 1/5 of the length from the upper end to the lower end of the second partition wall 9b.
  • one open end of the liquid supply pipe 14 was connected to the bottom of the phase separation chamber 8 and communicated with the lower phase liquid 6, and the other open end of the liquid supply pipe 14 communicated with the lower phase liquid storage chamber 11. Furthermore, the height of the upward bent portion 12 of the liquid supply pipe 14 (the height of the highest part of the pipe peripheral wall) was a height spaced downward from the upper end of the first partition wall 9a by an interval of 1/10 of the length from the upper end of the first partition wall 9a to the lower end of the first partition wall 9a. Furthermore, the open end of the branch portion 13 communicated with the gas phase portion of the phase separation tank 4 at a position 50 cm higher than the upper end of the first partition wall 9a.
  • crude IPA was supplied to the phase separation chamber 8 via the first supply pipe at a flow rate of 0.3 m/s.
  • the residence time of the mixture of crude IPA and azeotropic agent in the phase separation chamber 8 was 25 minutes.
  • benzene was supplied as an azeotropic agent via the fourth supply pipe 17 in an amount of 90 parts by mass per 100 parts by mass of crude IPA supplied to the phase separation chamber 8, causing phase separation into an upper phase liquid 5 containing the azeotropic agent, water, and IPA, and a lower phase liquid 6 containing water and IPA.
  • the upper phase liquid 5 formed in the phase separation chamber 8 overflowed the upper end of the first partition wall 9a and flowed into the upper phase liquid storage chamber 10.
  • the lower phase liquid 6 formed in the phase separation chamber 8 was sent to the lower phase liquid storage chamber 11 via the liquid delivery pipe 14.
  • the upper phase liquid 5 that flowed into the upper phase liquid storage chamber 10 had a composition of 26% IPA and 1% water by mass, and the water content was significantly reduced compared to the crude IPA.
  • the upper phase liquid 5 was supplied to the raw material supply stage of the azeotropic distillation tower 2 via the second supply pipe at a flow rate of 59 L/h and subjected to azeotropic distillation.
  • the azeotropic distillation column 2 is a packed column with a packing height of 100 cm, and it was confirmed through experiments that the theoretical number of plates is 35.
  • a condenser 3 is provided at the top of the azeotropic distillation column 2. Taking into account the flow rate of the upper phase liquid 5, the azeotropic distillation column 2 is designed to be small, with a diameter of 10 cm.
  • the temperature at the top of the column was 68°C, and the gauge pressure at the top of the column was 0 kPaG.
  • the first distillate containing an azeotropic mixture of benzene and water and IPA was supplied to the phase separation tank 4 via the third supply pipe 15 from the top of the azeotropic distillation column 2 and circulated, and the reflux amount of the first distillate was 59 L/h.
  • the composition of the first distillate was 68% by mass of benzene, 6% by mass of water, and 26% by mass of IPA.
  • the lower phase liquid 6 sent to the lower phase liquid storage chamber 11 was supplied to the IPA recovery distillation column 19 at 4 L/h via the fifth supply pipe 18 and distilled.
  • a second distillate containing an azeotropic mixture of IPA and water was extracted from the top of the IPA recovery distillation column 19 at 1.7 L/h and supplied to the phase separation tank 4 via a separately provided supply pipe. That is, in this embodiment, the second distillate was not extracted from the upper side of the IPA recovery distillation column 19.
  • a third distillate containing low boiling impurities was not extracted from the top of the IPA recovery distillation column 19 via the third extraction pipe 22.
  • a second bottoms containing water was extracted from the bottom of the IPA recovery distillation column 19 via the second extraction pipe 21.
  • the temperature of the top of the column was set to 85° C.
  • the gauge pressure of the top of the column was set to 10 kPaG.
  • the purified IPA extracted from the first extraction pipe 16 had a water content of 30 ppm and a purity (excluding the water content) of 99.99% by mass, making it a high-quality anhydrous IPA.
  • the flow rate of crude IPA was calculated to be 62 L/h, which was greater than the flow rate of upper phase liquid 5 in Example 1 (59 L/h).
  • the amount of heat consumed in the azeotropic distillation tower 2 was calculated to be 32.8 MJ/h, which was significantly greater than the amount of heat consumed in the azeotropic distillation tower 2 in Example 1 (23.7 MJ/h).
  • the diameter of the azeotropic distillation tower 2 was also calculated to need to be 12 cm, which was greater than the diameter of the azeotropic distillation tower 2 in Example 1 (10 cm).
  • first supply pipe 2 azeotropic distillation column 3; condenser 4; phase separation tank 5; upper phase liquid 6; lower phase liquid 7; second supply pipe 8; phase separation chamber 9a; first partition wall 9b; second partition wall 10; upper phase liquid storage chamber 11; lower phase liquid storage chamber 12; upward bent portion 13; branching portion 14; liquid transfer pipe 15; third supply pipe 16; first withdrawal pipe 17; fourth supply pipe 18; fifth supply pipe 19; IPA recovery distillation column 20; sixth supply pipe 21; second withdrawal pipe 22; third withdrawal pipe

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Thermal Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé de production d'alcool isopropylique purifié par déshydratation d'alcool isopropylique brut contenant de l'eau en tant qu'impureté, le procédé comprenant : une étape de séparation de phase qui consiste à stocker un liquide mixte d'alcool isopropylique brut et d'un agent azéotropique dans un réservoir de séparation de phase et à le séparer en phase en un liquide en phase supérieure contenant l'agent azéotropique, de l'eau et de l'alcool isopropylique et un liquide en phase inférieure contenant de l'eau ; et une étape de distillation azéotropique qui consiste à soumettre le liquide en phase supérieure à une distillation azéotropique dans une colonne de distillation azéotropique, et à extraire un distillat contenant un mélange azéotropique de l'agent azéotropique et de l'eau et un produit de fond contenant de l'alcool isopropylique, le distillat étant fourni au réservoir de séparation de phase.
PCT/JP2024/040792 2023-12-01 2024-11-18 Procédé et dispositif de production d'alcool isopropylique purifié Pending WO2025115671A1 (fr)

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JP2025512053A JP7695493B1 (ja) 2023-12-01 2024-11-18 精製イソプロピルアルコールの製造方法および製造装置

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JPS359024B2 (fr) * 1955-02-07 1960-02-07
JPS58134041A (ja) * 1982-02-01 1983-08-10 バスフ　アクチェン　ゲゼルシャフト 連続蒸留によるプロパノ−ルの製法
JPS61239628A (ja) * 1985-04-17 1986-10-24 Tokuyama Soda Co Ltd 半導体基材の洗浄方法
WO2023176192A1 (fr) * 2022-03-16 2023-09-21 株式会社トクヤマ Liquide de nettoyage de semi-conducteur et procédé de production de liquide de nettoyage de semi-conducteur

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US4139425A (en) * 1978-04-05 1979-02-13 R. O. Hull & Company, Inc. Composition, plating bath, and method for electroplating tin and/or lead

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Publication number Priority date Publication date Assignee Title
JPS359024B2 (fr) * 1955-02-07 1960-02-07
JPS58134041A (ja) * 1982-02-01 1983-08-10 バスフ　アクチェン　ゲゼルシャフト 連続蒸留によるプロパノ−ルの製法
JPS61239628A (ja) * 1985-04-17 1986-10-24 Tokuyama Soda Co Ltd 半導体基材の洗浄方法
WO2023176192A1 (fr) * 2022-03-16 2023-09-21 株式会社トクヤマ Liquide de nettoyage de semi-conducteur et procédé de production de liquide de nettoyage de semi-conducteur

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