WO2007034825A1 - Procede de separation solide-liquide et separateur solide-liquide - Google Patents

Procede de separation solide-liquide et separateur solide-liquide Download PDF

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Publication number
WO2007034825A1
WO2007034825A1 PCT/JP2006/318614 JP2006318614W WO2007034825A1 WO 2007034825 A1 WO2007034825 A1 WO 2007034825A1 JP 2006318614 W JP2006318614 W JP 2006318614W WO 2007034825 A1 WO2007034825 A1 WO 2007034825A1
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WO
WIPO (PCT)
Prior art keywords
liquid
solid
crystal
liquid separation
washing
Prior art date
Application number
PCT/JP2006/318614
Other languages
English (en)
Japanese (ja)
Inventor
Motoharu Kinoshita
Makoto Katsui
Hideki Murata
Original Assignee
Kyowa Hakko Kogyo 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 Kyowa Hakko Kogyo Co., Ltd. filed Critical Kyowa Hakko Kogyo Co., Ltd.
Priority to JP2007536521A priority Critical patent/JPWO2007034825A1/ja
Publication of WO2007034825A1 publication Critical patent/WO2007034825A1/fr

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Classifications

    • 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
    • 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
    • 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
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/30—Control equipment
    • 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
    • B01D21/30—Control equipment
    • B01D21/34—Controlling the feed distribution; Controlling the liquid level ; Control of process parameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0081—Use of vibrations, e.g. ultrasound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B11/00—Feeding, charging, or discharging bowls
    • B04B11/04—Periodical feeding or discharging; Control arrangements therefor
    • B04B11/043—Load indication with or without control arrangements
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering

Definitions

  • the present invention relates to a solid-liquid separation method and a solid-liquid separation device for obtaining a high-purity solid from a slurry containing a liquid and a solid.
  • crystallization by, for example, concentrated crystallization is performed.
  • a slurry containing the mother liquor and crystals is obtained, and the crystals are recovered by this slurry-force solid-liquid separation.
  • Centrifugal filtration is known as one of solid-liquid separation methods.
  • basket-type centrifugal filtration devices are widely used. During centrifugal filtration of the slurry, if the mother liquor is not sufficiently drained and remains attached to the crystals, the purity of the product will be reduced. So wash the mother liquor! Crystal washing is performed for the purpose of flowing.
  • a general basket-type centrifugal filtration device has a built-in program that uses a timer to transfer the process. After supplying the slurry, the mother liquor is removed for a certain period of time to separate the solid crystals and the liquid mother liquor. To do. After that, when moving to the crystal washing step, water or organic solvent such as methanol is sprayed on the crystal surface as a washing liquid from the washing nozzle attached to the centrifugal filtration device to wash away the adhering mother liquor. It has become. Cleaning is also performed by a timer, and the cleaning ends after a certain period of time. Then, remove the washing solution for a certain period of time. In some cases, washing and draining are repeated several times, and finally, the liquid is drained for a predetermined time to complete the crystal washing.
  • the crystal separation process ends without the mother liquor being sufficiently drained, adversely affecting subsequent processes such as drying and washing, and the purity decreases. Will get the crystal. If the mother liquor with large crystals is very good, it means that the centrifugal operation is continued despite the fact that the mother liquor has been drained, so that time is wasted.
  • JP-A-2004-231642 discloses a method for producing high-purity terephthalic acid by making the operation pressure at the time of centrifugation higher than the final crystallization pressure in the crystallization process by flash cooling.
  • Japanese Patent Laid-Open No. 2004-261710 discloses a method for separating and washing crystals by adjusting the crystal grain size to improve washing stability and washing efficiency. It should be considered to detect the liquid state and end the crystal separation process in an ideal state, or to move to the cleaning process.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2004-231642
  • Patent Document 2 JP 2004-261710 A
  • An object of the present invention is to recover a solid from a slurry containing a liquid and a solid by solid-liquid separation. In the process of draining liquid to collect, improve the washing efficiency of solids by sensing the liquid draining state and ending the solid separation process at an appropriate time, or moving to the solid washing process It is in.
  • the present invention provides (1) a slurry force containing a liquid and a solid by solid-liquid separation.
  • the slurry washing step including the liquid and the solid by the solid-liquid separation in the above (1) may be performed before or after the step of removing the liquid.
  • the slurry containing liquid and solid is not particularly limited, and examples thereof include a slurry containing mother liquor and crystals.
  • the liquid removal state of the mother liquor is sensed by the solid-liquid separation method used, and the crystal separation process is completed at an optimal time, or the process moves to the crystal washing process.
  • the mother liquor does not remain in the crystal, and salts contained in the mother liquor are not precipitated on the crystal surface by an excessive liquid removal step.
  • acoustic emission an acoustic emission (hereinafter referred to as acoustic emission) is generated when the mother liquor is desorbed by solid-liquid separation. , Abbreviated as “AE”), it was found that the mother liquor was accurately removed.
  • AE is defined as a signal in the frequency band in the ultrasonic range of several kHz to several MHz that is generated when the strain energy stored in the material is released as an elastic wave.
  • AE measurement is performed for non-destructive inspection.
  • AE measurement has various measurement items such as the number of AEs generated, frequency, or energy.
  • the AE value when the AE value is minimized, it can be accurately determined that the mother liquor is completely drained. Therefore, by measuring AE, it becomes possible to finish the crystal separation process at an appropriate time when the AE value is minimum for any crystal form. In addition, in the crystal separation method including the crystal washing step, it is possible to shift to the washing step at an appropriate time before the AE value is minimized.
  • the measurement value obtained by the AE sensor also senses the liquid removal state of the mother liquor, so that the timing for ending the crystal separation that depends on the size of the crystals is adequate. It is characterized by determining to.
  • the crystal separation method including the crystal washing process, should detect the desorption state of the mother liquor based on the measured value of the AE sensor and proceed to the washing process just before the mother liquor on the crystal surface is dehydrated. It is characterized by high cleaning efficiency V and crystal cleaning.
  • the present invention relates to the following (1) to (12).
  • a solid-liquid separation apparatus including means for removing liquid from a slurry containing liquid and solid by solid-liquid separation, and means for sensing the liquid removal state.
  • Solid-liquid separation including means for removing liquid from a slurry containing liquid and solid by solid-liquid separation, means for washing the solid separated using the washing liquid, and means for sensing the liquid's liquid removal state apparatus.
  • a sensing device comprising means for desorbing liquid from a slurry containing liquid and solid by solid-liquid separation, and means for sensing the liquid desorption state using an acoustic emission sensor.
  • the liquid drainage state is accurately sensed.
  • the time required to separate the solids can be optimized.
  • the cleaning efficiency when performing solid cleaning, the cleaning efficiency can be improved and a high-purity solid can be obtained.
  • FIG. 1 is a flowchart of a centrifugal filtration process for solid-liquid separation of crystals from a slurry.
  • ⁇ 2 Schematic showing the configuration of the apparatus of the present invention.
  • FIG. 3 is a schematic diagram illustrating a specific example of crystal separation and cleaning according to the present invention.
  • FIG. 4 is a schematic diagram illustrating a specific example of crystal separation and cleaning according to the present invention.
  • FIG. 5 is a graph showing an example of AE measurement values.
  • the solid-liquid separation device of the present invention is not particularly limited as long as it is a device capable of solid-liquid separation, and preferably a crystal separation device. Further, the solid-liquid separation device of the present invention includes a device having a solid-liquid cleaning function, preferably a crystal cleaning function.
  • the solid-liquid separation device of the present invention comprises a centrifugal filtration device 1 and an AE data analysis unit 2 as shown in FIG.
  • the centrifugal filtration device 1 shown in Fig. 2 is a general basket type centrifugal filtration device, but is not limited thereto.
  • the main body of the centrifugal filtration device 1 includes an outer tank 10 and an inner tank 11.
  • the outer tub 10 is fixed to a casing (not shown), and the inner tub 11 is a rotating cylinder provided with a large number of minute holes and can be rotated at a high speed.
  • the centrifugal filtration device 1 further includes a slurry supply port 12 for supplying the slurry 3 shown in FIG. 3 into the inner tank 11, and is separated from the slurry 3 by centrifugal filtration.
  • a crystal washing nozzle 13 for spraying the washing liquid 4 for washing the crystal 30 formed, and a filtrate outlet 14 for discharging the filtrate 31 of the mother liquor or washing liquid separated by centrifugal filtration are installed.
  • An AE sensor 15 for detecting a signal generated when the filtrate 31 drained from the slurry 3 by centrifugal filtration collides with the inner wall of the outer tank 10 is attached to the outer wall of the outer tank 10.
  • the AE sensor 15 is connected to the AE data analysis unit 2.
  • the detected signal is sent to the AE data analysis unit 2 for analysis.
  • the AE data analysis unit 2 is, for example, a personal computer with a built-in AE dedicated board for capturing AE signals and analyzing the data.
  • the measured value of the signal measured by the AE sensor can be displayed on the display.
  • the method of the present invention moves from the crystal separation step to the washing step according to the step shown in FIG. 1, and the crystal is washed.
  • each process proceeds with a timer after slurry supply, but in the method of the present invention, the timing of shifting from the mother liquor draining to the cleaning is determined by the measured value of the AE sensor. By doing so, it became possible to finish the crystal separation at the optimum time and to perform ideal cleaning.
  • the time is arbitrarily changed according to the dehydrated state, so that it is optimal for any crystal form. Crystal separation can be completed at a certain time, and even when the crystal is washed, it is possible to always proceed to the washing step in an ideal state. In addition, useless time can be saved, leading to shortening of the centrifugal filtration process time.
  • the process of separating the slurry force crystals by the method of the present invention and the process of shifting to this process force crystal washing process will be specifically described.
  • the slurry 3 containing the crystal 30 and the mother liquor is fed from the slurry feed port 12 into the inner tank 11 (FIG. 3a).
  • the inner tank 11 is rotated, and the centrifugal separation of the slurry 3 is started.
  • the crystal 30 is attached to the inner wall of the inner tank 11 by centrifugal force, while the mother liquor is drained into the outer tank 10 as a filtrate 31 through a number of micropores provided in the inner tank 11 (FIG. 3b).
  • the rotation of the inner tank 11 was started.
  • the slurry 3 can also be fed at a rotational speed. It is preferable to supply the slurry to the rotating inner tank, because the crystals are uniformly attached to the inner wall of the inner tank 11 and the cleaning efficiency is improved.
  • a conical protrusion can be provided at the center of the bottom of the inner tank 11 for the purpose of dispersing the slurry uniformly when the slurry is supplied.
  • the filtrate 31 that has been drained collides with the inner wall of the outer tank 10 to generate a signal.
  • the signal generated at this time is detected by the AE sensor 15 and sent to the data analysis unit 2.
  • the AE sensor 15 When only crystal separation is performed, if it is determined that the devolatilization is completed according to the analysis result of the AE signal, the rotation of the inner tank 11 is stopped and the crystal separation is terminated.
  • the cleaning liquid 4 is sprayed onto the crystal surface from four cleaning nozzles (FIG. 3c). After spraying the cleaning solution 4 for the set time of the timer, spraying is terminated (Fig. 4a). After the spraying of the cleaning liquid is completed, if it is determined that the liquid removal has been completed according to the analysis result of the AE signal from the filtrate 31 (in this case, the cleaning liquid), the rotation of the inner tank 11 is stopped and the liquid removal is completed. ( Figure 4b). If necessary, repeat the washing and draining steps ( Figure 3c and Figure 4a) to finish draining.
  • FIG. 5 shows an example of AE measurement during the centrifugal filtration operation by the method of the present invention.
  • the AE measurement value increases simultaneously with the slurry supply.
  • the mother liquor always collides with the inner wall of the centrifugal filtration device, so the AE measurement value shows a high value.
  • the mother liquor is gradually drained, and the amount of mother liquor that collides with the inner wall of the centrifugal filtration device decreases, so the AE measurement value also decreases.
  • the sprayed cleaning liquid is drained, and the AE measurement value rises again. If the spraying of the cleaning liquid is interrupted and the liquid removal process is started, the AE measurement value decreases. Repeat this several times (C area). After washing is completed, the liquid is finally drained (D region), and crystals are collected.
  • the force showing the minimum AE value (approx. 0.015V) in the dehydration process in the C region and in the final stage of the D region Therefore, if the minimum AE value is grasped in advance, salts contained in the mother liquor may precipitate on the crystal surface due to an excessive liquid removal process that does not leave a large amount of mother liquor remaining in the crystal during washing. It is possible to more accurately determine the most suitable state.
  • the appropriate time to complete the above-mentioned crystal separation process and the appropriate time to move from the liquid removal process to the washing process are the state and amount of slurry to be liquid removed, the substances contained, the target crystal purity, and the solid / liquid used. Depends on the separation device.
  • the solid to be separated or washed according to the present invention may be any solid that can be separated from the liquid by a solid-liquid separation device.
  • natural products such as amino acids, peptides, nucleic acid-related substances, etc. Examples of chemical compositions.
  • the slurry used in the present invention may be any slurry as long as it is a mixture of the above-described substance crystals and liquid.
  • the cells are obtained from the amino acid fermentation broth.
  • a solution obtained by concentrating the separated filtrate and precipitating the amino acid as crystals can be exemplified.
  • L-parin crystals were precipitated by concentrated crystallization from the filtrate obtained by separating the cells from the L-parin fermentation broth. Thereafter, the crystals and the mother liquor were separated by a basket type centrifugal filtration device (manufactured by Tanabe Wiltech Co., Ltd.) equipped with an AE sensor (Win-PCI2 system manufactured by Nippon Physical Acco Status Co., Ltd.).
  • a basket type centrifugal filtration device manufactured by Tanabe Wiltech Co., Ltd.
  • AE sensor Win-PCI2 system manufactured by Nippon Physical Acco Status Co., Ltd.
  • the crystal is colored when heat is applied to the mother liquor adhering to the crystal.
  • the degree of coloration of the heated crystal is measured, the amount of the mother liquor adhering to the crystal can be quantified, and the washing efficiency of the crystal can be quantified.
  • L-parin crystals finally obtained by each method in Table 1 were heated for 1 hour or 24 hours in a 105 ° C dry heat oven. Measure the absorbance (OD) at 430 nm of a 25 g ZL solution obtained by dissolving heated L-parin crystals in deionized water and color the value.
  • L-leucine crystals finally obtained by each method were dried at 60 ° C under vacuum for about 12 hours.
  • the method of the present invention 0.0.282

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Centrifugal Separators (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)

Abstract

L’invention concerne un procédé de séparation solide-liquide permettant d'atteindre une grande efficacité de séparation solide-liquide, et un séparateur solide-liquide, plus précisément un procédé de séparation solide-liquide caractérisé en ce que lors de l'étape d'élimination d'un liquide d'une pâte comprenant un liquide et un solide par séparation solide-liquide, le degré d’élimination du liquide est suivi afin de déterminer le moment de discontinuation de la séparation solide-liquide ; et un séparateur solide-liquide comprenant un moyen d’élimination d’un liquide d'une pâte comprenant un liquide et un solide par séparation solide-liquide et un moyen de suivi du degré d’élimination du liquide.
PCT/JP2006/318614 2005-09-22 2006-09-20 Procede de separation solide-liquide et separateur solide-liquide WO2007034825A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2007536521A JPWO2007034825A1 (ja) 2005-09-22 2006-09-20 固液分離方法および固液分離装置

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2005276106 2005-09-22
JP2005-276106 2005-09-22

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WO2007034825A1 true WO2007034825A1 (fr) 2007-03-29

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WO (1) WO2007034825A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018122216A (ja) * 2017-01-30 2018-08-09 日立造船株式会社 汚泥脱水装置、汚泥脱水装置の制御方法およびプログラム
EP3421136A1 (fr) * 2017-06-30 2019-01-02 Bjarne Christian Nielsen Holding ApS Système et procédé de commande de séparation de phases solides et liquides
CN114733227A (zh) * 2022-04-20 2022-07-12 河南精康制药有限公司 一种用于曲克芦丁结晶母液的回收利用装置及方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6680357B2 (ja) * 2016-06-30 2020-04-15 株式会社島津製作所 容器セットおよびそれを用いた試料調製方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61213098A (ja) * 1985-03-15 1986-09-22 株式会社東芝 脱水機の制御装置
JPS63260593A (ja) * 1987-04-16 1988-10-27 シャープ株式会社 脱水機の制御装置
JP2001017888A (ja) * 1999-07-09 2001-01-23 Matsushita Electric Ind Co Ltd 脱水乾燥装置
JP2001321697A (ja) * 2000-05-15 2001-11-20 Matsumoto Kikai Seisakusho:Kk 遠心ろ過方法
JP2002343763A (ja) * 2001-05-16 2002-11-29 Oomiya Kogyo Kk 半導体ウエハ用遠心分離機

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61213098A (ja) * 1985-03-15 1986-09-22 株式会社東芝 脱水機の制御装置
JPS63260593A (ja) * 1987-04-16 1988-10-27 シャープ株式会社 脱水機の制御装置
JP2001017888A (ja) * 1999-07-09 2001-01-23 Matsushita Electric Ind Co Ltd 脱水乾燥装置
JP2001321697A (ja) * 2000-05-15 2001-11-20 Matsumoto Kikai Seisakusho:Kk 遠心ろ過方法
JP2002343763A (ja) * 2001-05-16 2002-11-29 Oomiya Kogyo Kk 半導体ウエハ用遠心分離機

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018122216A (ja) * 2017-01-30 2018-08-09 日立造船株式会社 汚泥脱水装置、汚泥脱水装置の制御方法およびプログラム
EP3421136A1 (fr) * 2017-06-30 2019-01-02 Bjarne Christian Nielsen Holding ApS Système et procédé de commande de séparation de phases solides et liquides
CN114733227A (zh) * 2022-04-20 2022-07-12 河南精康制药有限公司 一种用于曲克芦丁结晶母液的回收利用装置及方法
CN114733227B (zh) * 2022-04-20 2024-03-12 河南精康制药有限公司 一种用于曲克芦丁结晶母液的回收利用装置及方法

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JPWO2007034825A1 (ja) 2009-03-26
TW200716246A (en) 2007-05-01

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