US20150165340A1 - Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor - Google Patents

Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor Download PDF

Info

Publication number
US20150165340A1
US20150165340A1 US14/123,764 US201314123764A US2015165340A1 US 20150165340 A1 US20150165340 A1 US 20150165340A1 US 201314123764 A US201314123764 A US 201314123764A US 2015165340 A1 US2015165340 A1 US 2015165340A1
Authority
US
United States
Prior art keywords
solution
storage tank
tryptophan
heating medium
temperature
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.)
Abandoned
Application number
US14/123,764
Other languages
English (en)
Inventor
Jong Pal Hong
Chil Won Lee
Hee Wan Lee
Gyeong Rye Choi
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.)
Laminar Co Ltd
Original Assignee
Laminar 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
Priority claimed from KR1020120097027A external-priority patent/KR101427324B1/ko
Priority claimed from KR1020120107996A external-priority patent/KR101372811B1/ko
Application filed by Laminar Co Ltd filed Critical Laminar Co Ltd
Publication of US20150165340A1 publication Critical patent/US20150165340A1/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
    • B01D9/0054—Use of anti-solvent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0063—Control or regulation
    • 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
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
    • C07D209/04—Indoles; Hydrogenated indoles
    • C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
    • C07D209/14—Radicals substituted by nitrogen atoms, not forming part of a nitro radical
    • C07D209/16—Tryptamines
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
    • C07D209/04—Indoles; Hydrogenated indoles
    • C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
    • C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D2009/0086—Processes or apparatus therefor
    • B01D2009/009—Separation of organic compounds by selective or extractive crystallisation with the aid of auxiliary substances forming complex or molecular compounds, e.g. with ureum, thioureum or metal salts
    • B01D2009/0095—Separation of organic compounds by selective or extractive crystallisation with the aid of auxiliary substances forming complex or molecular compounds, e.g. with ureum, thioureum or metal salts with the aid of other complex forming substances than ureum, thioureum or metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00033—Continuous processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00103—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor in a heat exchanger separate from the reactor

Definitions

  • the present invention relates to a purification system comprising a continuous reactor. More particularly, the present invention relates to a purification system configured such that a solution stored in a solution storage tank is dispersed/stirred ultrasonically and sent by an air compressor to a reactor in which the sent solution and a solvent introduced through another pathway are stirred to produce a reaction product, and a purification method using the purification system.
  • organic materials need to be purified.
  • organic materials that are used for organic light-emitting devices are pure target components separated from synthesized materials and are used for thin film deposition. With improvement in technology for purifying organic materials, the luminous efficiency of organic light-emitting devices is improved and the life span is also extended.
  • Tryptophan is an essential amino acid.
  • Conventional technologies for purification of tryptophan include methods disclosed in Japanese Patent Laid-Open Publication Nos. 1983-895, 1984-39857 and 1986-126070.
  • Japanese Patent Laid-Open Publication No. 1986-126070 has a problem in that, particularly when a reaction solution, prepared by a fermentation process and containing large amounts of impurities, is heated at a temperature of 95 ⁇ 100° C. in the presence of activated carbon, the amount of a degraded and colored substance increases because tryptophan contains an unstable indole ring in its structure.
  • It is an object of the present invention to provide an ultrahigh-purity purification system comprising a continuous reactor and configured such that a solution stored in a solution storage tank is dispersed/stirred ultrasonically and sent through an air compressor to a reactor in which the sent solution and a solvent introduced through another pathway are stirred to produce a reaction product and such that an organic material for use in organic light-emitting devices can be produced with an ultrahigh purity of 99.9% or higher in large amounts.
  • Another object of the present invention is to provide an system for purifying tryptophan, which adopts a method of dissolving tryptophan in an acidic or basic solution and then adding a counter solution thereto to neutralize the pH to thereby precipitate tryptophan, and which uses a continuous reactor to enable continuous production and increase the production rate by at least three times compared to conventional methods and the recovery rate and purity of tryptophan, and also which uses a polymer material as an additive to increase the density of particles so as not to be easily broken.
  • a purification system comprises: a solution storage tank configured to store a solution; an ultrasonic disperser configured to ultrasonically disperse particles contained in the solution in the solution storage tank; a stirrer configured to stir the solution stored in the solution storage tank; a heating jacket provided outside the solution storage tank and configured to control the internal temperature of the storage tank; an air compressor configured to suck the solution from the solution storage tank and send the sucked solution to a position next thereto; and a reactor configured to be supplied with the solution sent by the air compressor together with a solvent sent through a separate pathway and to stir the supplied solutions at high speed to continuously produce a reaction product having uniform particles.
  • an organic material for use in organic light-emitting devices can be produced with ultrahigh purity in large amounts.
  • an organic material having an ultrahigh purity of 99.9% or higher can be obtained.
  • an organic electroluminescent device When an organic electroluminescent device is fabricated using the organic material having increased purity as described above, the occurrence of dark spots in the device can reduce, the electrical and optical properties of the device can be improved, and the lifespan of the device can be extended.
  • a continuous reactor is used to increase the recovery rate of tryptophan by about 10% compared to that of convention methods, enable continuous production so as to increase the production rate by at least three times, and increase the purity of tryptophan to 99.9% or higher.
  • a polymer material is added to increase the density of particles so as not to be easily broken.
  • FIG. 1 shows the configuration of an ultrahigh-purity purification system according to the present invention.
  • FIG. 2 shows the detailed configuration of a continuous reactor that is included in the purification system of the present invention.
  • FIG. 3 shows the configuration of a cylinder in a continuous reactor that is included in the purification system of the present invention.
  • FIG. 4 shows the configuration of a system for purifying tryptophan according to another embodiment of the present invention.
  • FIG. 5 is a flow chart showing a method for purifying tryptophan according to the present invention.
  • FIGS. 6 to 8 are photographs showing the change in crystals as a function of the injection rate of sulfuric acid in a method for purifying tryptophan according to the present invention.
  • FIG. 9 shows a particle size distribution as a function of reaction time in a method for purifying tryptophan according to the present invention.
  • FIGS. 10 to 13 are photographs showing the shape of tryptophan crystals as a function of reaction time in a method for purifying tryptophan according to the present invention ( FIG. 10 : 1 hour, FIG. 11 : 6 hours, FIG. 12 : 26 hours, and FIG. 13 : 52 hours).
  • FIG. 14 is a graphic diagram showing the change in particle size as a function of the dissolution concentration of tryptophan in a method for purifying tryptophan according to the present invention.
  • FIG. 15 is a graphic diagram showing the change in recovery rate as a function of the dissolution concentration of tryptophan in a method for purifying tryptophan according to the present invention.
  • FIG. 16 is a graphic diagram showing the change in recovery rate as a function of the dissolution concentration of tryptophan in a method for purifying tryptophan according to the present invention.
  • FIGS. 17 and 18 are photographs showing the change in particle shape as a function of stirring speed in a method for purifying tryptophan according to the present invention ( FIG. 17 : 100 rpm, and FIG. 14 : 300 rpm).
  • FIG. 19 is a graphic diagram showing the change in particle size as a function of stirring speed in a method for purifying tryptophan according to the present invention
  • a purification system comprising a reactor according to the present invention comprises a solution storage tank, an ultrasonic disperser, a stirrer, a heating jacket and an air compressor.
  • the purification system may optionally comprise a filter, a separator, a dewaterer, a dryer or the like.
  • the purification system shown in FIGS. 1 to 3 comprises a reactor.
  • This purification system comprises a solution storage tank 100 , an ultrasonic disperser 200 , an air compressor 300 , a filter cartridge 400 , a temperature controlling unit 500 , a continuous reactor 600 , an organic material separator 700 , an organic material storage chamber 800 and a correction module 900 .
  • the solution storage tank 100 serves to store a solution of an organic material (OLED) in an organic solvent.
  • the concentration of the organic material in the organic solvent is preferably 100 g/L or lower, and if the concentration of the organic material is higher than the upper limit of the above concentration range, a crystallization reaction will be delayed or it will be difficult to obtain the desired purity.
  • organic material refers to any material that is provided between the anode and cathode of an organic electroluminescent device. Examples of an organic material or organometallic material that is used in an organic electroluminescent device include a light-emitting host material and host material, hole injection/transport materials, electron injection/transport materials, and hole/electron blocking layer materials.
  • the heating jacket 110 filled with a heating medium is provided outside the solution storage tank 100 so that the solution in the solution storage tank 100 can be heated up to 350 to dissolve the organic material in the organic solvent.
  • the solution storage tank 100 may further include a stirrer in order to uniformly mix the organic material with the organic solvent.
  • the ultrasonic disperser 200 is included in the solution storage tank 100 and serves to apply ultrasonic waves to the organic material to grind and decompose the organic material to thereby form nanoparticles. Because the organic material is not easily dissolved only by heating, it needs to be forcibly ground in order to increase the efficiency at which it is dissolved.
  • the ultrasonic disperser converts a frequency voltage of 50-60 Hz to high-frequency electrical energy of 20 kHz or higher in an oscillator called a generator, and the high-frequency electrical energy is converted to mechanical vibration by a piezoelectric ceramic material in a converter.
  • This conversion is known as the inverse piezoelectric effect, and the vertical vibration generated thereby is transferred to the liquid sample.
  • expansion negative pressure
  • shrinkage positive pressure
  • the air compressor 300 serves to suck the solution from the solution storage tank 100 and send the sucked solution to the filter cartridge 400 that is a position next thereto. If the temperature of the high-temperature solution is lowered while the solution is sent, the solution is precipitated as crystals, and in order to prevent this phenomenon, the solution should be sent in a pressurized state using the air compressor.
  • a pump may also be used in place of the air compressor, but in this case, crystals can be precipitated as described above, and for this reason, the air compressor is preferably used, as long as a solution to the precipitation problem is not provided.
  • the filter cartridge 400 serves to filter out fine impurities contained in the solution sent by the air compressor 300 and to decolorize the salt or ionic substance produced during the synthesis reaction.
  • the filter cartridge 400 comprises a filter case 410 and a material 420 filled in the filter case 410 , wherein the filled material may consist of one or a mixture of two or more selected from the group consisting of metal oxides, including activated alumina, silica, and titanium oxide, and natural stones, including activated carbon, bentonite, acid clay, and diatomaceous earth.
  • metal oxides including activated alumina, silica, and titanium oxide
  • natural stones including activated carbon, bentonite, acid clay, and diatomaceous earth.
  • the temperature controlling unit 500 serves to increase the temperature of the filter cartridge 400 to prevent crystals from being precipitated in the solution.
  • the temperature controlling unit 500 comprises a casing 510 enclosing the filter cartridge 400 , a heating medium 520 filled in the casing 510 , and a heater 530 for heating the heating medium 520 .
  • the continuous reactor 600 is configured to be supplied with the filtered solution that passed through the filter cartridge 400 together with a semi-solvent stored in a semi-solvent storage tank 10 by a pump P and to stir the supplied solution and semi-solvent to produce a reaction product having uniform particles.
  • the continuous reactor 600 comprises a cylinder 610 , a heating medium-filled chamber 620 , a partitioning plate 630 , a temperature controlling element 640 , a stirring body 650 , a stirring motor 660 , a belt pulley 670 and a belt 671 .
  • the cylinder 610 of the continuous reactor 600 has a reaction chamber 611 that receives the filtered solution and the semi-solvent, and in order to introduce the semi-solvent into the reaction chamber 611 , a semi-solvent injection port 611 a is formed at the upper portion of the cylinder 610 .
  • a solution injection port 611 b for introducing the organic material solution is formed at the lower portion of the cylinder 620 .
  • Reference numeral 611 c indicates a discharge port through which the reaction product is discharged after completion of the reaction.
  • the heating medium-filled chamber 620 is formed along the outer circumference of the reaction chamber 611 in a ring shape and is filled with a heating medium for controlling the temperature of the solution and semi-solvent received in the reaction chamber 611 .
  • the heating medium-filled chamber 620 is divided into a plurality of chambers by a plurality of partitioning plates 630 that are made of a thermal insulating material in order to prevent the heat exchange between the heating media filled in the plurality of heating medium-filled chambers 620 .
  • the temperature gradient of the solution passing through the reaction chamber 611 can be reduced.
  • the temperature gradient can change depending on the temperature of the heating medium.
  • Each of the heating medium-filled chambers 620 may further include a temperature sensor 621 serving to sense the temperature of the heating medium in each of the chambers and transmit the sensed temperature to an analysis and correction module 900 .
  • the temperature controlling element 640 serves to control the temperature of the heating medium and may, for example, be a circulator or a heater.
  • the stirring body 650 has a rod shape, is rotatably provided in the cylinder 610 and serves to stir the solution and semi-solvent received in the cylinder 610 .
  • mixing in the axial direction of the stirring body 650 decreases, and mixing in the radial direction increases.
  • the unstable fluid forms the so-called Taylor vortex in the form of a pair of rings rotating in opposite directions along the direction of the stirring body 650 .
  • This Taylor vortex can be used for fluid stability, because turbulent flow can be created by changing the rotating speed of the stirring body 650 .
  • the stirring motor 660 is disposed below the cylinder 610 and serves to provide a rotating force to the stirring body 650 .
  • the stirring motor 660 may be a speed-changeable stirring motor whose rotating speed can be controlled in the range of 10-2000 rpm by a direct voltage controller (not shown).
  • the rotating speed of the stirring body 650 that is rotated by the stirring motor 660 can also be changed in the above range (10-2000 pm) to cause turbulent flow in the solution.
  • the stirring motor 660 and the stirring body 650 are connected indirectly to each other by the belt pulley 670 and the belt 671 .
  • the stirring body 650 is maintained at a high temperature because the high internal temperature of the cylinder 610 is conducted thereto. Thus, if the high temperature of the stirring body is transferred directly to the stirring motor 660 , the life span of the stirring motor 660 can be shortened. For this reason, the stirring body 650 is connected indirectly to the stirring motor 660 by the belt 671 in order to block heat transfer therebetween.
  • the connection of the stirring body to the stirring motor by the belt has been described by way of example, the connection is not limited by the belt, and the connection can be achieved by a chain or a gear.
  • the wall surface of the reaction chamber 611 and the heating medium-filled chamber 620 may be coated with Teflon 622 in order to provide corrosion resistance to the wall surface.
  • Teflon 622 may also be made of hastelloy-C.
  • Hastelloy-C is an acid-resistant alloy having a very high corrosion resistance, and thus when it is applied to a portion that frequently contacts a chemical solution, such as the cylinder 610 of the present invention, it can provide corrosion resistance.
  • the organic material separator 700 is connected to the discharge port 611 c of the continuous reactor 600 and serves to separate the slurry-type reaction product, discharged from the continuous reactor 600 , into a solid organic material and a liquid.
  • the organic material storage chamber 800 serves to store the solid organic material separated by the organic material separator 700 .
  • the analysis and correction module 900 serves to collect the liquid separated by the organic material separator 700 , and then analyze whether or not the state of the collected liquid is normal and correct the process conditions into optimal process conditions on the basis of the analyzed data.
  • the correction function can be controlled by a computer.
  • the system for purifying tryptophan comprises a filter 10 for filtering solids, a storage tank 20 , a heating tank 30 , an air compressor 40 , a continuous reactor 50 , a dewaterer 60 and a dryer 70 .
  • the filter 10 for filtering solids is configured to filter out solids from a tryptophan solution while allowing the solution to pass through the filter.
  • the filter 10 has a mesh size (or pore size) of 0.1 ⁇ m or larger, and preferably 0.1-0.5 ⁇ m, so that it filters out solids having a size of 0.5 ⁇ m or larger from the tryptophan solution and allows only fine solids having a size of less than 0.5 ⁇ m to pass therethrough.
  • the filter 10 performs a first purification step.
  • the storage tank 20 serves to store the tryptophan solution that passed through the filter 10 .
  • the storage tank 20 includes a temperature sensor 21 so that the temperature of the tryptophan solution stored in the storage tank 20 can be sensed in real time.
  • the heating jacket 30 is provided outside the storage tank and functions to control the internal temperature of the storage tank 20 .
  • the heating jacket 30 is filled with a heating medium and provided in such a manner that a portion of the storage tank 20 is placed in the heating jacket 30 such that the tryptophan solution in the storage tank 20 can be controlled to a suitable temperature by heating the heating medium by a heat source.
  • the air compressor 40 functions to suck the tryptophan solution from the storage tank 20 and send the sucked solution to a position next thereto.
  • a pump may be provided in place of the air compressor.
  • the continuous reactor 50 is configured to be supplied with the tryptophan solution sent by the air compressor 40 together with sulfuric acid sent through a separate pathway and to stir the supplied solutions to continuously produce a reaction product.
  • the continuous reactor is as described above, and thus the detailed description thereof is omitted.
  • the dewaterer 60 is connected to the discharge port of the continuous reactor and functions to separate a liquid from a slurry-type reaction product discharged from the continuous reactor. It may be a centrifugation-type dewaterer.
  • a method for purifying tryptophan according to the present invention is performed in the following order (see FIG. 5 ).
  • Step 1 is a solid removal step (S 10 ).
  • the tryptophan solution is passed through a filter to remove solids having a size larger than a predetermined size, before it is stored in the storage tank.
  • the filter that is used in the solid removal step preferably has a mesh size (or pore size) of 0.1-0.5 ⁇ m.
  • a mesh size or pore size
  • Step 2 is a pH adjusting step (S 20 ).
  • caustic soda NaOH
  • the pH is preferably adjusted to 3-11.
  • Step 3 is a temperature controlling step (S 30 ).
  • the temperature of the tryptophan solution is controlled to a suitable temperature using the heating jacket provided outside the storage tank.
  • Step 4 is a density increasing step (S 40 ).
  • a polymer material is added to the tryptophan solution in the storage tank to increase the density of particles in the tryptophan solution. This step is performed using the continuous reactor.
  • the polymer material may be any one selected from among PVA (polyvinyl alcohol), carrageenan, alginic acid, and gelatin.
  • PVA polyvinyl alcohol
  • carrageenan polyvinyl alcohol
  • alginic acid alginic acid
  • gelatin gelatin
  • the size of crystals increases with the passage of time, and the growth rate of tryptophan crystals is higher than that in the case in which no polymer is added.
  • an acid solution particularly sulfuric acid solution
  • particles in the tryptophan solution grow to a size of about 300 ⁇ m or larger.
  • the particles are easily broken by sonication due to their low strength, but the strength of the particles is increased when a polymer material having a low molecular weight is added thereto.
  • Step 5 is a supply step (S 50 ).
  • the tryptophan solution in the storage tank is continuously supplied to the continuous reactor.
  • the supply of the tryptophan solution can be automatically performed by the air compressor or the like.
  • Step 6 is a crystal precipitation step (S 60 ).
  • an acid solution (particularly sulfuric acid solution) is added to the tryptophan solution introduced into the continuous reactor to neutralize the pH of the tryptophan solution to thereby precipitate crystal particles.
  • the tryptophan solution is an amphoteric substance that easily dissolves in an acidic or basic solution, and thus this tryptophan solution is dissolved in an acidic or basic solution, after which a counter solution is added thereto to neutralize the pH, thereby precipitating crystals.
  • the tryptophan solution is dissolved in a sodium hydroxide solution, and then an acidic solution is added thereto.
  • Step 7 is a solid-liquid separation step (S 70 ).
  • the crystal particles that precipitated in the continuous reactor are dewatered by the dewaterer, thereby separating the crystals into a solid and a liquid.
  • the resulting tryptophan having a high water content is introduced into a centrifugation-type dewaterer, and the dewaterer is operated to reduce the water content to 60% or lower.
  • a suitable dewatering time is determined by performing dewatering for any amount of time, collecting the dewatered tryptophan sludge, measuring the water content of the sludge, and adjusting the dewatering time based on the measurement results.
  • the rotating speed of the dewaterer is 5,000-12,000 rpm, and the dewatering time is 50-60 minutes. If the rotating speed is lower than 500 rpm, the dewatering time will be too long, and if the rotating speed is higher than 12,000 rpm, the dewatering rate will not significantly differ from that in the case in which the rotating speed is lower than 12,000 rpm, and thus the efficiency of dewatering will be reduced.
  • Step 8 is a drying step (S 80 ).
  • the dewatered tryptophan sludge cake still has a high water content, the water content is lowered to 10% or less by hot-air drying to form powder.
  • a process of washing the sludge cake and separating the washing water by centrifugation may further be performed. This powdering process provides high-purity tryptophan.
  • Tryptophan concentration 200 g/L
  • Injection rate of sulfuric acid 0.5 mL/min, 2 mL/min, and injection at a time.
  • FIGS. 6 to 8 are microscopic photographs of 1, 2 and 3 in Table 1 above.
  • Tryptophan concentration 100 g/L
  • Amount and rate of injection of sulfuric acid 100 mL & 16.7 mL/min;
  • the recovery rate was about 95% or higher without significantly changing depending on the reaction time, suggesting that tryptophan precipitated within a short time.
  • Tryptophan concentration 10, 100 and 200 g/L;
  • lowering the dissolution concentration of tryptophan is a method capable of inhibiting nucleation and that the method of the present invention is suitable for lowering nucleation. It is believed that as nucleation decreases, nuclei are attached to dissolved tryptophan to cause crystal growth.
  • Tryptophan concentration 10 g/L
  • the material of this Experiment is a sheet-like material comprising particles having a weak bonding strength therebetween.
US14/123,764 2012-09-03 2013-01-17 Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor Abandoned US20150165340A1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
KR1020120097027A KR101427324B1 (ko) 2012-09-03 2012-09-03 연속식 반응기를 포함하는 초고순도 정제장치
KR10-2012-0097027 2012-09-03
KR1020120107996A KR101372811B1 (ko) 2012-09-27 2012-09-27 트립토판 정제장치 및 방법
KR10-2012-0107996 2012-09-27
PCT/KR2013/007885 WO2014035211A1 (ko) 2012-09-03 2013-09-02 연속 반응기를 포함하는 정제 장치 및 이 연속식 반응기를 이용한 정제 방법

Publications (1)

Publication Number Publication Date
US20150165340A1 true US20150165340A1 (en) 2015-06-18

Family

ID=50183933

Family Applications (2)

Application Number Title Priority Date Filing Date
US14/123,764 Abandoned US20150165340A1 (en) 2012-09-03 2013-01-17 Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor
US14/635,925 Active 2034-10-28 US9937480B2 (en) 2012-09-03 2015-03-02 Purification apparatus including continuous reactors and purification method using continuous reactors

Family Applications After (1)

Application Number Title Priority Date Filing Date
US14/635,925 Active 2034-10-28 US9937480B2 (en) 2012-09-03 2015-03-02 Purification apparatus including continuous reactors and purification method using continuous reactors

Country Status (4)

Country Link
US (2) US20150165340A1 (ja)
EP (1) EP2893964B1 (ja)
JP (1) JP6352919B2 (ja)
WO (1) WO2014035211A1 (ja)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150196890A1 (en) * 2012-09-03 2015-07-16 Laminar Co.,Ltd Purification apparatus including continuous reactors and purification method using continuous reactors
US10601035B2 (en) 2013-06-14 2020-03-24 Posco Method of preparing core-shell particles
CN113582913A (zh) * 2021-08-18 2021-11-02 河北广祥制药有限公司 一种连续精制硝苯地平的方法
CN114797547A (zh) * 2022-06-07 2022-07-29 重庆新申新材料股份有限公司 一种高纯度锶化合物、钡化合物溶液生产用加液装置

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014084547A1 (ko) * 2012-11-27 2014-06-05 (주)라미나 혼합용 반응 장치 및 이 반응 장치를 이용한 제조 방법
WO2015147487A1 (ko) * 2014-03-28 2015-10-01 주식회사 디엠에스 이온성 액체를 이용한 유기재료 정제 방법 및 장치
CN105396530A (zh) * 2014-09-12 2016-03-16 天津法莫西医药科技有限公司 一种用于制备生物制剂的生化反应装置
CA3148236A1 (en) 2019-07-22 2021-01-28 Canopy Growth Corporation Continuous crystallization of cannabinoids in a stirred-tank reactor

Family Cites Families (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2725219A (en) * 1953-02-16 1955-11-29 Firth George Reactor
US3004013A (en) * 1954-04-28 1961-10-10 Detrex Corp Method for producing finely divided polyvinyl chloride
US3892539A (en) * 1969-09-26 1975-07-01 Merck & Co Inc Process for production of crystals in fluidized bed crystallizers
JPS58895A (ja) 1981-06-26 1983-01-06 Mitsui Toatsu Chem Inc Ｌ−トリプトフアンの製造方法
DE3132421A1 (de) * 1981-08-17 1983-02-24 Hoechst Ag, 6000 Frankfurt Kontinuierliches verfahren zur herstellung von vinylchloridpolymerisaten in waessriger suspension
JPS5939857A (ja) 1982-08-28 1984-03-05 Ajinomoto Co Inc アミノ酸の晶析方法
JPS60237054A (ja) * 1984-05-10 1985-11-25 Nippon Kayaku Co Ltd アミノ酸の晶析法
JPS61126070A (ja) 1984-11-21 1986-06-13 Mitsui Toatsu Chem Inc Ｌ−トリプトフアンの脱色精製方法
JPH0648990B2 (ja) * 1987-01-14 1994-06-29 味の素株式会社 トリプトフアンの精製方法
JP3273118B2 (ja) * 1995-04-20 2002-04-08 東北電力株式会社 高圧処理装置
US6906172B2 (en) * 1998-03-10 2005-06-14 Large Scale Biology Corporation Flexible processing apparatus for isolating and purifying viruses, soluble proteins and peptides from plant sources
US6306658B1 (en) * 1998-08-13 2001-10-23 Symyx Technologies Parallel reactor with internal sensing
US6471392B1 (en) * 2001-03-07 2002-10-29 Holl Technologies Company Methods and apparatus for materials processing
JP2001199957A (ja) * 2000-01-13 2001-07-24 Ajinomoto Co Inc トリプトファンの晶析法
IL149932A0 (en) * 2002-05-30 2002-11-10 Nano Size Ltd High power ultrasonic reactor and process for ultrasonic treatment of a reaction material
JP4178909B2 (ja) * 2002-10-24 2008-11-12 東亞合成株式会社 アクリルアミドアルカンスルホン酸溶液の製造方法
US7488464B2 (en) * 2003-07-31 2009-02-10 Enviroscrub Technologies Corporation Metal oxide processing methods and systems
KR100550942B1 (ko) * 2003-12-29 2006-02-13 제일모직주식회사 유기물질의 정제장치 및 정제방법
US20100124583A1 (en) * 2008-04-30 2010-05-20 Xyleco, Inc. Processing biomass
KR101007430B1 (ko) * 2008-06-09 2011-01-12 경희대학교 산학협력단 용해도 조절에 의한 거대 결정입자의 제조방법
JP5011437B2 (ja) * 2008-06-10 2012-08-29 ケイエヌディティ アンド アイ カンパニー，リミテッド 巨大結晶粒子の成長のための結晶化反応装置及びこれを含む結晶分離工程システム
KR100974324B1 (ko) * 2008-09-26 2010-08-06 고등기술연구원연구조합 유기성 슬러지로부터 고체 고형물과 액상 탈리액을 함유하는 고액 슬러리를 제조하는, 유기성 슬러지의 연속식처리 장치
US8420841B2 (en) * 2009-09-15 2013-04-16 Texas Tech University System Methods and systems to produce biodiesel fuel
JP2013516297A (ja) * 2010-01-08 2013-05-13 プレジデント アンド フェロウズ オブ ハーバード カレッジ バイオフィルム処理のための方法およびコーティング
US20150165340A1 (en) * 2012-09-03 2015-06-18 Laminar Co., Ltd. Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150196890A1 (en) * 2012-09-03 2015-07-16 Laminar Co.,Ltd Purification apparatus including continuous reactors and purification method using continuous reactors
US9937480B2 (en) * 2012-09-03 2018-04-10 Laminar Co., Ltd Purification apparatus including continuous reactors and purification method using continuous reactors
US10601035B2 (en) 2013-06-14 2020-03-24 Posco Method of preparing core-shell particles
CN113582913A (zh) * 2021-08-18 2021-11-02 河北广祥制药有限公司 一种连续精制硝苯地平的方法
CN114797547A (zh) * 2022-06-07 2022-07-29 重庆新申新材料股份有限公司 一种高纯度锶化合物、钡化合物溶液生产用加液装置

Also Published As

Publication number Publication date
US20150196890A1 (en) 2015-07-16
WO2014035211A1 (ko) 2014-03-06
US9937480B2 (en) 2018-04-10
EP2893964A1 (en) 2015-07-15
JP6352919B2 (ja) 2018-07-04
EP2893964A4 (en) 2016-05-25
JP2015535725A (ja) 2015-12-17
EP2893964B1 (en) 2019-11-27

Similar Documents

Publication Publication Date Title
US20150165340A1 (en) Purification System Comprising Continuous Reactor and Purification Method Using Continuous Reactor
US10875783B2 (en) Method for continuously preparing nano zinc oxide with membrane reactor
EP3235787A1 (en) Device for producing lithium sulfide, and method for producing lithium sulfide
CN113244793B (zh) 一种耐用高通量乳液分离膜材料的制备及应用
KR20180064707A (ko) 고순도 나노 알루미나의 제조방법
CN216170061U (zh) 一种硫酸乙烯酯的升华结晶提纯装置系统
CN105219385A (zh) 一种pH稳定的强发光的碳量子点的制备方法
KR101427324B1 (ko) 연속식 반응기를 포함하는 초고순도 정제장치
CN106966382A (zh) 一种超临界连续水热合成石墨烯量子点的方法
KR100733957B1 (ko) 연속식 용석 결정화 분리방법
CN104528954B (zh) 一种可降解复合生物填料的制备方法
KR100733969B1 (ko) 연속식 용석 결정화 분리장치
Fan et al. The controlled growth of calcium sulfate dihydrate (gypsum) in aqueous solution using the inhibition effect of a bubble column evaporator
CN108047472A (zh) 一种基于石墨烯量子点掺杂的聚合物复合薄膜的制备方法
CN101787541B (zh) 一种cim膜法除硝的方法
CN112850862B (zh) 氯离子去除材料Ti3C2Tx/BiOCl及制备方法和应用
CN112341629A (zh) 使用内循环旋转填充床制备纳米金属-有机框架材料的方法
CN114685480A (zh) 一种精制及粉碎利伐沙班原料药的方法
KR100721868B1 (ko) 쿠에트-테일러 반응기를 이용한 구아닐산나트륨 결정화공정 시스템
Gashi et al. Effect of the modification time of coal with aryldiazonium salts on the performance of cellulose–acetate coal heterogeneous reverse osmosis membranes
KR101372811B1 (ko) 트립토판 정제장치 및 방법
CN104190355A (zh) 多孔炭材料的制备方法及其用于处理含油污水的处理方法
CN211688870U (zh) 一种壬二酸氢铵制备系统
CN205517753U (zh) 一种工业化制备功能化石墨烯的反应装置
JP5780580B2 (ja) 精製粘土製造方法

Legal Events

Date Code Title Description
STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION