WO2022107812A1 - 精製装置 - Google Patents

精製装置 Download PDF

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Publication number
WO2022107812A1
WO2022107812A1 PCT/JP2021/042245 JP2021042245W WO2022107812A1 WO 2022107812 A1 WO2022107812 A1 WO 2022107812A1 JP 2021042245 W JP2021042245 W JP 2021042245W WO 2022107812 A1 WO2022107812 A1 WO 2022107812A1
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WO
WIPO (PCT)
Prior art keywords
tank
line
crystallization
mother liquor
solid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/042245
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English (en)
French (fr)
Japanese (ja)
Inventor
章吾 荒井
真志 迎
裕貴 和田
隼也 福本
敬幸 松田
豊文 酒井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Shokubai Co Ltd
Original Assignee
Nippon Shokubai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Shokubai Co Ltd filed Critical Nippon Shokubai Co Ltd
Priority to CN202180077924.XA priority Critical patent/CN116457331A/zh
Priority to KR1020237020173A priority patent/KR102928219B1/ko
Priority to EP21894686.1A priority patent/EP4249095B1/en
Priority to US18/253,684 priority patent/US20240010600A1/en
Priority to JP2022563802A priority patent/JP7635258B2/ja
Publication of WO2022107812A1 publication Critical patent/WO2022107812A1/ja
Anticipated expiration legal-status Critical
Priority to ZA2023/05911A priority patent/ZA202305911B/en
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/26—Separation of sediment aided by centrifugal force or centripetal force
    • B01D21/262—Separation of sediment aided by centrifugal force or centripetal force by using a centrifuge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • B01D9/0045—Washing of crystals, e.g. in wash columns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/02—Crystallisation from solutions
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B63/00—Purification; Separation; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C57/00—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
    • C07C57/02—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
    • C07C57/03—Monocarboxylic acids
    • C07C57/04—Acrylic acid; Methacrylic acid

Definitions

  • the present invention relates to a purification apparatus that can be suitably used for purifying industrially produced compounds.
  • a cooling crystal tank having a clarification portion at the upper part and a rigid purification tower having a clarification part at the upper part and a heater at the lower part are connected in series to purify crystals produced in the crystal tank.
  • the crystals sent from the crystal tank are sent in order to the side of the crystal tank connected to the above, and the crystals sent from the crystal tank are gravity-precipitated in the purification tower, and a part of the crystals heated and melted by the heater at the bottom of the purification tower is raised as a reflux liquid.
  • a purification method for cleaning crystals by contacting them with gravity-precipitated crystals is disclosed (see Patent Documents 1 and 2).
  • the suspension containing the acrylic acid crystals and the crude acrylic acid melt produced in the crystallization tank is sent to the washing column, the crystals are forcibly transported in the washing column, and the crystals are melted at the lower part of the column.
  • a method for purifying acrylic acid for washing crystals in a washing column using the melt obtained in the above method as a washing liquid is disclosed (see Patent Document 3).
  • a purification method for increasing the purity of acrylic acid by repeating suspension crystallization or layered crystallization a plurality of times from an aqueous solution containing acrylic acid is disclosed (see Patent Document 4).
  • the present inventor has studied a purification apparatus capable of obtaining a high-purity compound at high yield and low cost, and N crystallization tanks or aging tanks including at least one crystallization tank are connected in series.
  • a purification device having a structure in which the most upstream crystallization tank or aging tank is connected to a washing column, at least one of the lines for sending the slurry from the crystallization tank or the aging tank to the upstream tank is a solid-liquid separation device.
  • a line for directly sending the mother liquor from the next upper tank and one upstream tank for the mother liquor via the solid-liquid separator are provided in each of the 1st to N-1st tanks of the crystallization device.
  • the present invention is a compound purification device having a crystallization device having a crystal forming unit and a washing column for forcibly transporting crystals
  • the crystallization device has N (N ⁇ 2) tanks.
  • the first tank is downstream and the Nth tank is upstream, and they are connected in series.
  • At least the first tank is a crystallization tank equipped with a cooling mechanism, and the second and subsequent tanks are crystallization tanks.
  • it is an aging tank, and at least one tank has a line for supplying a liquid to be purified containing a compound
  • the washing column has a line for carrying out the product and a line for returning the mother liquor to the crystallization apparatus.
  • the line to be returned to the crystallization device is connected to at least the Nth tank, and the crystallization device is a line for supplying the slurry from the Nth tank to the washing column, and a tank one upstream from the downstream tank. It has a line to send the slurry to the liquid and a line to send the mother liquid from the upstream tank to each of the 1st to N-1st tanks, and N-1 from the downstream tank to the upstream tank. At least one of the lines for sending the slurry is a line for sending the slurry to the tank one upstream via the solid-liquid separator, and the mother liquor from which the crystals have been removed by the solid-liquid separator is the original.
  • the purification apparatus includes at least one of the lines for supplying the mother liquor from the tank to the mother liquor via the solid-liquid separation apparatus, and further has a line for sending the mother liquor to the outside of the purification apparatus.
  • All of the 1st to N-1st tanks included in the crystallization device have a line for sending the slurry to the tank one upstream via the solid-liquid separation device and a mother liquor discharged from the solid-liquid separation device. It is preferable to have a line for returning at least a part of the above to the original tank.
  • At least one is a line that sends the mother liquor from the upstream tank via the solid-liquid separator. Is preferable.
  • At least one of the solid-liquid separation devices provided in the line for sending the slurry from the downstream tank to the upstream tank is one that sends the mother liquor in addition to the line for returning the mother liquor to the original tank. It is preferable to have the above additional line, and the additional line is connected to the downstream tank and / or the outside of the purification apparatus with respect to the original tank.
  • At least one of the 1st to N-1st tanks included in the crystallization apparatus has a line for directly sending the mother liquor from the tank one upstream.
  • the cooling mechanism is preferably of a type that cools the contents of the tank outside the tank.
  • the cleaning column may or may not have a mechanical mechanism for scraping the crystal bed.
  • the compound is preferably (meth) acrylic acid.
  • the line that sends the slurry from at least the N-1st tank to the Nth tank is a solid-liquid separator.
  • the solid-liquid separation device provided in the line for sending the slurry from the N-1st tank to the Nth tank is a basket-type centrifugal separation line, which is a line for sending the slurry to the tank one upstream via the liquid. It is preferably a machine or a decanter type centrifuge.
  • the compound purification apparatus of the present invention produces a high-purity compound in a high yield even when purifying an organic compound that produces crystals having a relatively small particle size or when purifying a crude compound solution having a low purity. Therefore, it can be obtained by reducing the amount of crystallization residue discharged. Moreover, since the amount of cleaning liquid in the cleaning column can be reduced, the operating cost of the device can be reduced.
  • the purification apparatus of the present invention has a crystallization apparatus in which N (N ⁇ 2) tanks are connected in series and a washing column for forcibly transporting crystals, and at least the first tank included in the crystallization apparatus is It is a crystallization tank equipped with a cooling mechanism, the second and subsequent tanks are crystallization tanks or aging tanks, the Nth tank is connected to the washing column, and the slurry is transferred from the downstream tank to the upstream tank in order. The liquid is sent, and the slurry is sent from the Nth tank to the washing column.
  • At least one of the lines for sending the slurry from the downstream tank to the upstream tank in order is a line for sending the slurry to the upstream tank via the solid-liquid separation device, and is discharged from the solid-liquid separation device. It has a line to return at least a part of the slurry to the original tank.
  • all of the 1st to N-1st tanks included in the crystallization apparatus are a line for directly sending the mother liquor from the tank one upstream, and the solid-liquid separation from the tank one upstream. It has at least one of the lines for sending the mother liquor via the apparatus, and further has a line for sending the mother liquor to the outside of the purification apparatus.
  • the line for sending the mother liquor to the outside of the purification apparatus is preferably a line for sending the mother liquor from the most downstream tank to the outside of the purification apparatus, thereby the most downstream tank.
  • the low-purity mother liquor (crystallization residue) enriched with impurities can be discharged in a smaller amount, and a high-purity compound can be obtained in a high yield.
  • the washing column of the liquid obtained by heating and melting the purified crystals, a part of the liquid is used as a washing liquid and brought into countercurrent contact with the crystal bed to increase the purity of the crystals.
  • the amount of this cleaning liquid can be reduced by supplying it to the cleaning column. As a result, the amount of crystals generated in the crystallization tank can be reduced, and the operating cost of the refrigerator can be reduced.
  • the mother liquor is brought into countercurrent contact with the crystals and the liquid level of each tank is adjusted.
  • a line is required to send the crystal-free mother liquor from the upstream side to the downstream side, and from the tank inside the purification equipment to the outside of the purification equipment (preferably from the most downstream tank to the outside of the purification equipment). ..
  • a crystal sedimentation region is provided in the upper part of the tank, from which a crystal-free mother liquor (hereinafter, may be referred to as a clear mother liquor) is overflowed from the upstream to the downstream side of the tank, and the most.
  • a method of directly discharging the waste from the downstream tank to the outside of the purification device is known. This method does not require a liquid feed pump and has the advantage that the liquid level of each tank can be easily adjusted, but the tank structure is complicated because a crystal sedimentation region is required in the upper part of each tank.
  • the sedimentation rate of the crystals is slow, so it is necessary to make the tank itself excessively large in order to design the sedimentation region. .. If the crystals are too fine to form the sedimentation region well, the crystals will be sent to the downstream side, and there is a problem that the purification effect as an apparatus is reduced.
  • At least one of the lines for sending the slurry from the downstream tank to the upstream tank in order is a line for sending the slurry to the upstream tank via the solid-liquid separation device.
  • the ratio of the line that sends the slurry to the one upstream tank via the solid-liquid separator is 60% or more. It is preferable to have. Most preferably, 100%, that is, all of the N-1 lines that feed the slurry from the downstream tank to the upstream tank, feed the slurry to the upstream tank via the solid-liquid separator. It is a line to do. Further, of the lines for sending the slurry from the downstream tank to the upstream tank, at least one line for sending the slurry from the N-1st tank to the Nth tank is via the solid-liquid separator. It is preferable that the line is for sending the slurry to the upstream tank.
  • those having a line for sending the slurry to the tank one upstream via the solid-liquid separator has at least a part of the mother liquor discharged from the solid-liquid separator as the original.
  • the slurry containing the concentrated crystals which has a line to be returned to the tank and separated by the solid-liquid separator, is sent to the upstream tank, and at least a part of the remaining mother liquor is returned to the original tank. Will be done.
  • all of the 1st to N-1th tanks are lines for directly sending the mother liquor from the upstream tank and one upstream as a line for sending the mother liquor from the upstream tank to the tank. It has at least one of the lines for sending the mother liquor from the tank of the above via a solid-liquid separator. Having these lines makes it possible to keep the liquid level in the tank constant.
  • At least one of the 1st to N-1st tanks contained in the crystallization apparatus has a line for directly sending the mother liquor from the tank one upstream. More preferably, the N-1st tank has a line for directly feeding the mother liquor from the tank one upstream (Nth tank). The reason why it is preferable to have a line for directly sending the mother liquor from the Nth tank to the N-1st tank will be described later.
  • the tank included in the crystallization device has a line for sending the mother liquor from the one upstream tank via the solid-liquid separator, the crystals are sent from the one upstream tank to the downstream side. Since it can be effectively suppressed by solid-liquid separation, the purification efficiency of the purification device can be maintained high even when the purification device is used for purification of a compound having a slow crystal settling rate. Therefore, of the lines for sending the mother liquor from the upstream tank to each of the 1st to N-1th tanks, at least one is a line for sending the mother liquor from the upstream tank via the solid-liquid separator. Is preferable.
  • a line for sending mother liquor via a solid-liquid separator is provided in a tank one downstream from the tank included in the crystallization device, it is one upstream from the viewpoint of the cost of the purification device itself and the operating cost of the device. It is preferable to share the solid-liquid separation device provided in the line for sending the slurry to the tank. By doing so, the number of equipment of the solid-liquid separator and the liquid feed pump can be reduced.
  • one or more additional lines for further feeding the mother liquor are provided in the line for returning the mother liquor from the solid-liquid separation device provided in the line for sending the slurry to the tank one upstream.
  • the device may be configured such that the additional line is connected to a tank one downstream from the original tank. Further, the additional line may be further branched to connect to two or more downstream tanks in addition to one downstream tank with respect to the original tank. Further, the additional line may be connected to the outside of the purification device.
  • the crystallization device has such a configuration, that is, at least one of the solid-liquid separation devices provided in the line for sending the slurry from the downstream tank to the upstream tank returns the mother liquor to the original tank. It is the present invention that the return line has one or more additional lines for delivering the mother liquor, the additional lines being connected to the downstream tank and / or out of the purification apparatus with respect to the original tank. Is one of the preferred embodiments of the purification apparatus of.
  • the ratio of those having such an additional line is preferably 30% or more, more preferably 60. % Or more, more preferably 100%.
  • a basket-type centrifuge As the solid-liquid separator, commonly used devices such as a basket-type centrifuge, a decanter-type centrifuge, a liquid cyclone, and a filter can be used.
  • An example of a basket-type centrifuge is the Escha Wis-extruded centrifuge of Tsukishima Kikai Co., Ltd.
  • an example of a decanter-type centrifuge is a bird-decanter type centrifuge of Tsukishima Kikai Co., Ltd., and a screw of IHI Co., Ltd.
  • a decanter type centrifuge and the like can be mentioned.
  • the crystal concentration in the cake after solid-liquid separation is preferably 80% or more, more preferably 85% or more, still more preferably 90% or more.
  • the crystal concentration after concentration is preferably 40% or more, more preferably 50% or more, still more preferably 60% or more.
  • the crystal concentration in the concentrated slurry is preferably 25% or more, more preferably 30% or more, and more preferably 35% or more. If the slurry concentration is too high, the fluidity decreases and the risk of pipe blockage increases. Therefore, the slurry concentration after concentration is preferably 55% or less, more preferably 50% or less, still more preferably 45% or less.
  • the line for sending the slurry from at least the N-1st tank to the Nth tank is solid. It is preferable that the line is for sending the slurry to the tank one upstream via the liquid separation device, and in that case, it is provided in the line for sending the slurry from the N-1st tank to the Nth tank.
  • the solid-liquid separator is preferably a basket-type centrifuge or a decanter-type centrifuge.
  • the crystallization apparatus includes a plurality of crystallization tanks or aging tanks including at least one crystallization tank.
  • the total number of crystallization tanks and aging tanks is not particularly limited, but a basket-type centrifuge and a decanter-type centrifuge are used as the solid-liquid separator from the viewpoint of sufficiently improving the purity of crystals and mother liquor. In the case of 2 or more, in other cases, it is preferably 3 or more.
  • the effect of improving the purity of crystals and mother liquor increases as the number of tanks increases, but if it is too large, capital investment increases and the power consumption of pumps, stirrers, etc. attached to the tanks also increases, which is disadvantageous. Become. Therefore, the total number of crystallization tanks and aging tanks is preferably 6 or less regardless of the type of solid-liquid separation device. More preferably, it is 5 or less.
  • the other tanks may be a crystallization tank or an aging tank, but the number of aging tanks included in the crystallization device is 0. It is preferably up to two. More preferably, it is 0 to 1.
  • the tank included in the crystallization device preferably has a structure capable of forming a clear mother liquor layer on the upper part, and any one of the 1st to N-1st tanks included in the crystallization device is one.
  • the line is a line for directly feeding the clear mother liquor layer on the upper part of the upstream tank by overflow.
  • the line for sending the mother liquor to the outside of the purification apparatus is a line for sending the mother liquor to the outside of the purification apparatus by overflow.
  • the purification apparatus of the present invention preferably has a line for sending the mother liquor to the outside of the purification apparatus from the most downstream first tank included in the crystallization apparatus, but the line is included in the crystallization apparatus. It is one of the preferred embodiments of the purification apparatus of the present invention that the line is to send the clear mother liquor layer on the upper part of the first tank to the outside of the purification apparatus by overflow.
  • a solid-liquid separation device is installed to separate the mother liquor and crystals from the slurry taken out from the tank by the solid-liquid separation device.
  • One or more mother liquors can be sent to the downstream tank.
  • the mother liquor separated by the solid-liquid separation device may be discharged to the outside of the purification device, and the mother liquor is sent out of the purification device from the first tank included in the crystallization device via the solid-liquid separation device.
  • all the tanks preferably 30% or more, more preferably 60% or more, and most preferably N-1st, separate the mother liquor into a solid solution.
  • the structure is such that the liquid is sent to one downstream tank (or two or more downstream tanks in addition to the tank) via the device and / or discharged to the outside of the crystallization device. By doing so, the size of the tank can be reduced, and the investment amount and construction area can be reduced. Further, as described above, it is preferable that the solid-liquid separation device in this case is shared with the solid-liquid separation device provided in the line for sending the slurry to the tank one upstream from the viewpoint of cost.
  • the capacity is larger than that of the downstream tank in order to hold / mature the slurry to be sent to the washing column, and the purity of the slurry is improved and crystals are formed more than the downstream tank. Due to its large diameter and easy growth, it is relatively easy to design the crystal sedimentation region at the top of the tank, that is, the clear mother liquor layer. Therefore, it is preferable that the Nth tank has a structure in which the mother liquor is directly sent to the downstream tank by overflow.
  • the crystallization tank included in the crystallization apparatus of the present invention is provided with a cooling mechanism, and can cool a solution of a compound to precipitate crystals and generate a slurry containing crystals and a mother liquor.
  • a cooling jacket is attached to the tank itself to directly cool the inside of the tank to generate crystals, and a cooling mechanism is separated from the tank and connected by piping to generate cooling / crystals while circulating. It is roughly divided into.
  • the method in which the cooling jacket is attached to the tank itself has the advantage of reducing the number of devices, but in order to increase the heat transfer area, it is necessary to increase the size of the tank itself. If high production capacity is required, the size of the tank will be excessively large, which will be a disadvantage in terms of initial investment and site area.
  • the type in which the contents of the tank are cooled outside the tank is preferable.
  • the tank and the cooling mechanism are connected by a pipe, and a part of the solution of the compound (or the slurry containing crystals) in the tank is sent to the cooling mechanism to generate crystals in the cooling mechanism.
  • the heat transfer area can be easily increased by increasing the cooling mechanism, and the scale-up of the crystallization tank can be easily performed.
  • the cooling mechanism in this case is not particularly limited as long as it can cool the solution of the compound to precipitate crystals, but it is a shell & tube type heat exchanger and spiral that can secure a large heat transfer area. It is preferable to use a type heat exchanger or the like, a cooling disk type crystallizer that crystallizes while scraping the cooling surface, a scraping type cooling crystallizer or the like.
  • the cooling disk type crystallizer may be any as long as it cools the solution of the compound to precipitate crystals and scrapes the precipitated crystals, but it is composed of a tube and a plurality of cooling plates separating the inside thereof. It is possible to use a structure in which crystals are generated on the wall surface of the cooling plate and a stirring blade having a wiper is rotated inside the tube to scrape the crystals.
  • the scraping-type cooling crystallizer may be any as long as it cools the solution of the compound to precipitate crystals and scrapes the precipitated crystals, but it is composed of a double-structured tube, and the refrigerant is applied to the outer tube.
  • a solution of the compound in the tank (or a slurry containing crystals) is flowed through the inner tube to form crystals on the wall surface of the inner tube, and a shaft with a scraping blade is rotated inside the inner tube to crystallize.
  • a structure that scrapes off can be used.
  • the crystallization apparatus of the present invention may or may not have an aging tank, but it is preferable to have an aging tank.
  • the aging tank does not have a cooling mechanism for precipitating crystals, and is a tank for growing compound crystals by holding the compound crystals for a certain period of time.
  • the tank for sending the liquid to the washing column that is, the Nth tank is the aging tank.
  • the aging tank is not particularly limited as long as it can hold the crystal of the compound in a suspended state in the tank. By holding the crystals for a certain period of time, fine crystals are melted by Ostwald ripening, large crystals are further grown, the crystal diameter distribution is narrowed, and the purification efficiency in the washing column can be further improved. Further, even in the crystallization tank, the same effect as the aging tank can be expected by holding the crystals for a certain period of time.
  • a slurry containing compound crystals is sent from the Nth tank of the crystallization device to the washing column included in the purification apparatus of the present invention, and the crystals are washed to obtain high-purity compound crystals as a product. ..
  • the washing column of the preferred form in the present invention when the specific gravity of the crystals is larger than that of the mother liquor, the crystals move downward in the column to form a crystal bed. Then, at the lower part of the column, some crystals are extracted from the crystal bed while being suspended in a circulating solution (cleaning solution circulating in the cleaning column) and heated and melted, and a part of the circulating solution containing the obtained molten solution is extracted as a product. ..
  • a part of the remaining circulating liquid (washing liquid) is brought into countercurrent contact with the crystal bed to wash the crystals.
  • the mother liquor in the washing column is returned to the crystallization apparatus through a line for returning the mother liquor to the crystallization apparatus.
  • the line for returning the mother liquor to the crystallizer is connected to at least the Nth tank, but may be connected to a further downstream tank. Further, it may have a line for returning a part of the mother liquor to the washing column again.
  • the crystal moves upward in the column, and the crystal bed is suspended, melted, and the product is extracted at the upper part of the column, contrary to the above.
  • the cleaning column included in the purification apparatus of the present invention forcibly conveys the crystal bed.
  • a hydraulic cleaning column (hydraulic cleaning column) or the like for forming / transporting the slurry can be mentioned.
  • the operating principle of these cleaning columns is described in the book Melt Crystallization (Edited by Joachim Ullrich, Heike Grade, Shaker Verlag, Aachen 2003).
  • the washing column is not particularly limited as long as it can wash the crystals, and may be either a mechanical washing column or a hydraulic washing column.
  • Mechanical cleaning columns are characterized by high stability during operation and high compound purification efficiency.
  • the hydraulic cleaning column is characterized in that it has a high production capacity per column cross-sectional area, there are few driving parts in the cleaning column, and there are few troubles caused by the equipment. In purifying the easily polymerizable substance, it may be possible to suppress the generation of the polymer in the cleaning column by using a hydraulic cleaning column having few driving parts.
  • Preferred forms of the wash column include those having a mechanical mechanism for scraping the crystal bed (see US Pat. No. 3,872009A).
  • a washing column having a forced transport mechanism for a crystal bed a method is used in which the purified crystal bed is scraped off with a scraper or the like, resuspended, and then melted.
  • wash column is one that does not have a mechanical mechanism for scraping the crystal bed (see US Pat. No. 7,425273B2).
  • the crystal bed is scraped by the dynamic pressure of the circulating fluid. Since there is no sliding surface such as a shaft seal portion, the generation of a polymer due to liquid retention, sliding heat, etc. may be suppressed in the purification of easily polymerizable substances.
  • the solution of the compound as the liquid to be purified may be supplied to the purification apparatus of the present invention to any of the tanks contained in the crystallization apparatus, but from the viewpoint of purification efficiency, the second and subsequent tanks may be supplied. It is preferable to do this.
  • the optimum location varies depending on the supply liquid composition, crystallization yield, and crystal concentration efficiency in the solid-liquid separation device, and can be appropriately selected.
  • the crystallization temperature in the crystallization tank in the purification apparatus of the present invention may be appropriately adjusted according to the type of the compound to be purified, but is generally -1 to ⁇ 15 ° C., preferably ⁇ 15 ° C. with respect to the melting point of the pure substance.
  • the temperature is in the range of 1.5 to -13.5 ° C, more preferably ⁇ 3.5 ° C to -12.5 ° C, and even more preferably ⁇ 5 to -11.5 ° C.
  • the temperature is preferably 0 to 12 ° C. It is more preferably 1 to 10 ° C, still more preferably 2 to 8.5 ° C.
  • High-purity crystals are produced when the temperature of the crystallization tank is high.
  • the crystallization tank uses a scraping-type cooling crystallizer described later, it is suitable for crystal scraping in the crystallization tank.
  • problems such as the need for a large amount of power.
  • problems such as blocking of the scraping scraper may occur when the crystallization tank uses a scraping type cooling crystallizer, and operation may occur. It can be difficult to continue.
  • the temperature of the crystallization tank is high, it is necessary to reduce the temperature difference between the refrigerant and the crystallization tank and reduce the amount of crystals produced per heat transfer area. If the temperature of the crystallization tank is low, the purity of the produced crystals will decrease, but if the crystallization tank uses a scraping type cooling crystallizer, the power required for scraping the crystals in the crystallization tank can be small. Even if the temperature difference between the refrigerant and the crystallization tank is increased, scraper blocking is unlikely to occur. As a result, the temperature difference between the refrigerant and the crystallization tank can be increased, and the amount of crystals produced per heat transfer area can be increased. However, if the crystallization temperature is too low, the crystal grain size produced becomes fine and the crystals tend to be difficult to settle.
  • the residence time of the compound in the crystallization tank and the aging tank may be appropriately adjusted according to the type of the compound to be purified, but generally considering the yield of the compound obtained after purification, the efficiency of purification, and the capital investment cost. 0.02 to 6 hours.
  • the residence time is longer than a certain level in order to arrange the particle size distribution of the slurry to be sent to the washing column and reduce the reflux ratio (washing liquid flow rate / purified acrylic acid flow rate) in the washing column. It is preferably 0.5 to 6 hours, more preferably 1 to 5 hours, and even more preferably 1.2 to 4.5 hours.
  • the residence time is preferably 0.03 to 4 hours, more preferably 0.04 to 3 hours, still more preferably 0.05 to 2 hours, and most preferably 0.05 to 2 hours. 0.1 to 1.5 hours.
  • the residence time of the compound in the crystallization tank here means that when the crystallization tank is of a type that cools the contents of the tank described later outside the tank, it stays in the cooling mechanism inside and outside the tank. Means time to do.
  • the residence time of each tank is the combined capacity of the tank and the cooling mechanism outside the tank, the flow rate for supplying the slurry to the tank or washing column upstream from the tank, and the liquid from each tank to the lower tank or outside the purification device. It is calculated as the value obtained by dividing the flow rate of liquid delivery / discharge by the sum of the flow rates.
  • the purification apparatus of the present invention may be used for purification of any compound, but as described above, it can be suitably used for purification of crystals having poor precipitation property, and is therefore suitable for purification of (meth) acrylic acid. Can be used for. Therefore, it is one of the preferred embodiments of the present invention that the compound purified by the purification apparatus of the present invention is (meth) acrylic acid.
  • the solution of the compound used in the purification apparatus of the present invention is a (meth) acrylic acid aqueous solution or a crude (meth) acrylic acid solution.
  • the (meth) acrylic acid aqueous solution means a solution in which (meth) acrylic acid is dissolved in water.
  • the crude (meth) acrylic acid solution is a solution composed of (meth) acrylic acid and contains impurities such as by-products during the production of (meth) acrylic acid. These can be obtained, for example, by collecting the gas of the compound, which is a reaction product obtained by the gas phase oxidation reaction of propylene and isobutylene, in an absorption tower and distilling if necessary, but can be obtained by synthesizing it by itself.
  • a (meth) acrylic acid aqueous solution or a crude (meth) acrylic acid solution can be cooled, for example, to obtain a slurry containing crystals of (meth) acrylic acid.
  • Examples of the by-products include acids such as propionic acid, acetic acid, maleic acid, benzoic acid and acrylic acid dimer, aldehydes such as acrolein, furfural, formaldehyde and glyoxal, acetone and protoanemonin. ..
  • a solvent such as toluene or methyl butyl ketone may be contained.
  • (meth) acrylic acid is acrylic acid and / or methacrylic acid.
  • FIG. 1 shows an apparatus having one crystallization tank and one aging tank as a crystallization apparatus, and a line for directly sending the mother liquor from the aging tank, which is one upstream tank, is installed in the crystallization tank.
  • a line is installed to directly discharge the residue (mother solution) from the crystallization tank, which is the most downstream tank.
  • the solution 1 of the compound used in the purification apparatus is introduced into the aging tank 21.
  • the slurry containing the crystals cooled by the crystallization tank 11 in which the cooling mechanism is installed is sent to the solid-liquid separation device 31 by the line 51.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, the concentrated crystal slurry is sent to the adjacent aging tank 21 on the line 52, and the mother liquor is returned to the crystallization tank 11 on the line 61. .. Further, the residue 2 is discharged from the crystallization tank 11 to the outside of the purification apparatus on the line 71, and the liquid level of the crystallization tank 11 is adjusted. After growing the crystals in the aging tank 21, the crystal slurry is sent to the mechanical cleaning column 41 on the line 53. Further, in order to adjust the liquid level of the aging tank 21, the mother liquor is directly sent from the aging tank 21 to the crystallization tank 11 through the line 72.
  • the crystals are compacted by the piston to form a crystal bed. Then, the crystal bed is scraped off at the lower part of the column, suspended in a circulating solution, and melted by heating. A part of the circulating fluid containing the obtained melt is carried out as high-purity compound 3. A part of the remaining circulating liquid (cleaning liquid) is returned to the mechanical cleaning column 41 and brought into countercurrent contact with the crystal bed to clean the crystals. Further, the mother liquor in the washing column is returned to the aging tank 21 through the line 75 for returning the mother liquor to the crystallization apparatus. The compound is purified in this way, and a high-purity compound is obtained.
  • FIG. 2 shows a device having one crystallization tank and one aging tank as a crystallization device, and a line for directly feeding the mother liquor from the aging tank, which is one upstream tank, is installed in the crystallization tank.
  • a line is installed to directly discharge the residue (mother solution) from the crystallization tank, which is the most downstream tank.
  • the crystallization tank a tank in which the contents of the tank are cooled outside the tank is used.
  • the crystallization tank 11 is composed of a tank 11A and a cooling mechanism 11B outside the tank, and is connected by lines 111 and 121.
  • the solution of the compound (or the slurry containing the crystals of the compound) sent from the tank 11A to the cooling mechanism 11B on the line 111 is cooled by the cooling mechanism 11B, and the slurry containing the precipitated crystals is sent to the tank 11A on the line 121.
  • a part of the slurry containing the compound crystals is sent from the tank 11A to the cooling mechanism 11B by the line 111, and the rest is sent to the solid-liquid separation device 31 by the line 51.
  • FIG. 3 shows an apparatus having two crystallization tanks as a crystallization apparatus, in which a line for directly sending the mother liquor from the crystallization tank 12 which is one upstream tank is installed in the crystallization tank 11, and is the most downstream.
  • a line is installed to directly discharge the residue (mother solution) from the crystallization tank 11 which is a tank.
  • the cleaning column is hydraulic and has a mechanical mechanism for scraping the crystal bed.
  • the solution 1 of the compound used in the purification apparatus is introduced into the crystallization tank 12.
  • the crystallization tank 11 is composed of a tank 11A and a cooling mechanism 11B outside the tank, and is connected by lines 111 and 121.
  • the solution of the compound (or the slurry containing the crystals of the compound) sent from the tank 11A to the cooling mechanism 11B on the line 111 is cooled by the cooling mechanism 11B, and the slurry containing the precipitated crystals is sent to the tank 11A on the line 121.
  • a part of the slurry containing the compound crystals is sent from the tank 11A to the cooling mechanism 11B by the line 111, and the rest is sent to the solid-liquid separation device 31 by the line 51.
  • the crystallization tank 12 is also composed of a tank 12A and a cooling mechanism 12B outside the tank, and is connected by lines 112 and 122.
  • a part of the slurry containing the crystal of the compound is sent from the tank 12A to the cooling mechanism 12B by the line 112, and is returned to the tank 12A by the line 122.
  • the crystal slurry is sent from the crystallization tank 12 to the hydraulic cleaning column 42 by the line 53.
  • the crystal bed is scraped off by a mechanical mechanism (scraper), and the crystal bed is extracted while being suspended in the circulating fluid and melted by heating. It is carried out as compound 3 of.
  • a part of the remaining circulating liquid (cleaning liquid) is returned to the hydraulic cleaning column 42 and brought into countercurrent contact with the crystal bed to wash the crystals.
  • FIG. 4 shows a device having two crystallization tanks and one aging tank as a crystallization device, and a line for directly sending the mother liquor from one upstream tank is installed between the three tanks, and the most downstream. A line is installed to directly discharge the residue (mother solution) from the tank.
  • the slurry containing the crystals cooled by the crystallization tank 11 in which the cooling mechanism is installed is sent to the solid-liquid separation device 31 by the line 51.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, the concentrated crystal slurry is sent to the adjacent crystallization tank 12 on the line 52, and the mother liquor is returned to the crystallization tank 11 on the line 61. Is done. Further, the residue 2 is discharged from the crystallization tank 11 to the outside of the purification apparatus on the line 71, and the liquid level of the crystallization tank 11 is adjusted. In the crystallization tank 12, the same operation as in the crystallization tank 11 is performed, and the slurry containing the crystals is sent from the crystallization tank 12 to the solid-liquid separation device 32 along the line 53.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, the concentrated crystal slurry is sent to the adjacent aging tank 21 on the line 54, and the mother liquor is returned to the crystallization tank 12 on the line 62. .. Further, in order to adjust the liquid level of the crystallization tank 12, the mother liquor is directly sent from the crystallization tank 12 to the crystallization tank 11 through the line 72. After growing the crystals in the aging tank 21, the crystal slurry is sent to the mechanical cleaning column 41 on the line 55. Further, in order to adjust the liquid level of the aging tank 21, the mother liquor is directly sent from the aging tank 21 to the crystallization tank 12 through the line 73 connecting the aging tank 21 and the crystallization tank 12.
  • FIG. 5 shows a device having three crystallization tanks and one aging tank as a crystallization device, and a line for directly sending the mother liquor from one upstream tank is installed between the four tanks, and the most downstream.
  • a line is installed to directly discharge the residue (mother solution) from the tank.
  • the cleaning column is hydraulic and has a mechanical mechanism for scraping the crystal bed.
  • the solution 1 of the compound used in the purification apparatus is introduced into the crystallization tank 13.
  • the slurry containing crystals is sent from the crystallization tank 12, which is the second tank from the most downstream, to the solid-liquid separation device 32 along the line 53.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, the concentrated crystal slurry is sent to the adjacent crystallization tank 13 on the line 54, and the mother liquor is returned to the crystallization tank 12 on the line 62. Is done. Further, in order to adjust the liquid level of the crystallization tank 12, the mother liquor is directly sent from the crystallization tank 12 to the crystallization tank 11 through the line 72. The same operation as in the crystallization tank 12 is performed in the crystallization tank 13, and the slurry containing the crystals is sent from the crystallization tank 13 to the solid-liquid separation device 33 along the line 55.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, the concentrated crystal slurry is sent to the adjacent aging tank 21 on the line 56, and the mother liquor is returned to the crystallization tank 13 on the line 63. .. Further, in order to adjust the liquid level of the crystallization tank 13, the mother liquor is directly sent from the crystallization tank 13 to the crystallization tank 12 through the line 73. After growing the crystals in the aging tank 21, the crystal slurry is sent to the hydraulic cleaning column 42 on the line 57.
  • the mother liquor is directly sent from the aging tank 21 to the crystallization tank 13 through the line 74 connecting the aging tank 21 and the crystallization tank 13.
  • the crystal bed is scraped off by a mechanical mechanism (scraper), and the crystal bed is extracted while being suspended in the circulating fluid and melted by heating. It is carried out as compound 3 of.
  • a part of the remaining circulating liquid (cleaning liquid) is returned to the hydraulic cleaning column 42 and brought into countercurrent contact with the crystal bed to wash the crystals.
  • FIG. 6 shows a device having two crystallization tanks and one aging tank as a crystallization device, and a line for sending mother liquor from one upstream tank between three tanks via a solid-liquid separation device. Is installed, and a line is installed to discharge the residue from the most downstream tank via a solid-liquid separator.
  • a solid-liquid separation device 33 for separating the residue from the slurry in the crystallization tank is installed in place of the line for directly discharging the residue, and the slurry taken out from the crystallization tank 11 is provided.
  • the residue 2 separated by the solid-liquid separation device 33 is discharged to the outside of the purification device, the remaining crystals are returned to the crystallization tank 11, and the liquid in the crystallization tank 11 is discharged. The surface is adjusted.
  • a solid-liquid separation device 34 is installed in place of the line that directly sends the mother liquor to the crystallization tank 11, and the slurry taken out from the crystallization tank 12 is sent to the solid-liquid separation device 34 by the line 83.
  • the mother liquor sent and separated by the solid-liquid separation device 34 is sent to the crystallization tank 11 for liquid level adjustment, and the remaining crystals are returned to the crystallization tank 12.
  • a solid-liquid separation device 35 is installed in place of the line that directly sends the mother liquor to the crystallization tank 12, and the slurry taken out from the aging tank 21 is sent to the solid-liquid separation device 35 by the line 85.
  • the mother liquor separated by the solid-liquid separation device 35 is sent to the crystallization tank 12 for liquid level adjustment, and the remaining crystals are returned to the aging tank 21.
  • the cleaning column 43 is a hydraulic type and does not have a mechanical mechanism for scraping the crystal bed.
  • FIG. 7 shows a device having two crystallization tanks and one aging tank as a crystallization device, and a line for sending mother liquor from one upstream tank between three tanks via a solid-liquid separation device.
  • a line is installed to discharge the residue from the most downstream tank via the solid-liquid separator, and the mother liquor is separated from the slurry taken out from the second crystallization tank and discharged to the most downstream (
  • the slurry containing the crystals cooled by the crystallization tank 11 and precipitated is sent to the solid-liquid separation device 31 by the line 51.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, and the concentrated crystal slurry is sent to the adjacent crystallization tank 12 by the line 52.
  • a part of the mother liquor separated by the solid-liquid separation device 31 is returned to the crystallization tank 11 by the line 61, and the rest is discharged to the outside of the purification device by the additional line 101 connected to the line 61.
  • the slurry containing the crystals cooled and precipitated in the crystallization tank 12 is sent to the solid-liquid separation device 32 by the line 53.
  • the slurry is separated into a mother liquor and a concentrated crystal slurry, and the concentrated crystal slurry is sent to the adjacent aging tank 21 by the line 54.
  • a part of the mother liquor separated by the solid-liquid separation device 32 is returned to the crystallization tank 12 by the line 62, and the rest is sent to the crystallization tank 11 by the additional line 102 connected to the line 62.
  • the line 51 ⁇ solid-liquid separation device 31 ⁇ lines 61, 101 correspond to the line 81 ⁇ solid-liquid separation device 33 ⁇ lines 82, 91 in the device of FIG. 6, and the solid-liquid separation device 33 is installed. Instead, the number of devices is reduced by sharing the solid-liquid separation device 31 provided in the line for sending the slurry to the upstream tank.
  • line 53 ⁇ solid-liquid separation device 32 ⁇ line 62, 102 corresponds to line 83 ⁇ solid-liquid separation device 34 ⁇ lines 84, 92 in the device of FIG. 6, and instead of installing the solid-liquid separation device 34, The number of devices is reduced by sharing the solid-liquid separation device 32 provided in the line for sending the slurry to the upstream tank.
  • FIG. 8 shows a device having two crystallization tanks and one aging tank as a crystallization device, from the second crystallization tank to the most downstream (first) crystallization tank via a solid-liquid separation device.
  • a line for sending the mother liquor and a line for discharging the residue from the most downstream tank via the solid-liquid separator are installed, and a line for sending the mother liquor directly from the aging tank to the second crystallization tank is installed.
  • This is a solid-liquid separation device for separating the mother liquor from the slurry taken out from the second crystallization tank and sending it to the most downstream crystallization tank, and from the most downstream crystallization tank to the outside of the purification device.
  • the solid-liquid separation device for separating the discharged residue is shared with the solid-liquid separation device provided in the line for sending the slurry to the tank one upstream. Further, as the crystallization tank, a tank in which the contents of the tank are cooled outside the tank is used. Hereinafter, only the parts different from the purification apparatus of FIG. 7 will be described.
  • the crystallization tank 11 is composed of a tank 11A and a cooling mechanism 11B outside the tank, and is connected by lines 111 and 121.
  • the solution of the compound (or the slurry containing the crystals of the compound) sent from the tank 11A to the cooling mechanism 11B on the line 111 is cooled by the cooling mechanism 11B, and the slurry containing the precipitated crystals is sent to the tank 11A on the line 121.
  • a part of the slurry containing the compound crystals is sent from the tank 11A to the cooling mechanism 11B by the line 111, and the rest is sent to the solid-liquid separation device 31 by the line 51.
  • the crystallization tank 12 is also composed of a tank 12A and a cooling mechanism 12B outside the tank, and is connected by lines 112 and 122.
  • a part of the slurry containing the crystal of the compound is sent from the tank 12A to the cooling mechanism 12B by the line 112, and the rest is sent to the solid-liquid separation device 32 by the line 53.
  • the line 73 that sends the mother liquor directly from the aging tank 21 to the tank 12A. Have.
  • Line 91 The residue (mother liquid) separated from the slurry taken out from the tank by a solid-liquid separator is removed from the purification device.
  • Lines 92 and 93 The mother liquor separated from the slurry taken out from the tank by the solid-liquid separator is sent to the downstream tank by one line 101: The slurry taken out from the most downstream tank is separated by the solid-liquid separator.
  • Lines 111, 121, 112, 122 A line connecting the tank of the crystallization tank and the cooling mechanism, which cools the contents of the tank outside the tank.

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  • Crystallography & Structural Chemistry (AREA)
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PCT/JP2021/042245 2020-11-20 2021-11-17 精製装置 Ceased WO2022107812A1 (ja)

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CN202180077924.XA CN116457331A (zh) 2020-11-20 2021-11-17 纯化装置
KR1020237020173A KR102928219B1 (ko) 2020-11-20 2021-11-17 정제 장치
EP21894686.1A EP4249095B1 (en) 2020-11-20 2021-11-17 Purification device
US18/253,684 US20240010600A1 (en) 2020-11-20 2021-11-17 Purification device
JP2022563802A JP7635258B2 (ja) 2020-11-20 2021-11-17 精製装置
ZA2023/05911A ZA202305911B (en) 2020-11-20 2023-06-02 Purification device

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CN117229245B (zh) * 2023-09-18 2025-07-04 西安国康瑞金制药有限公司 一种科立内酯二醇的纯化方法

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JPWO2022107812A1 (https=) 2022-05-27
EP4249095A4 (en) 2024-11-20
CN116457331A (zh) 2023-07-18
EP4249095B1 (en) 2026-01-21
US20240010600A1 (en) 2024-01-11
TW202227177A (zh) 2022-07-16
KR20230109681A (ko) 2023-07-20
ZA202305911B (en) 2024-10-30

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