CN113289370A - DL-phenylalanine continuous crystallization purification method - Google Patents

DL-phenylalanine continuous crystallization purification method Download PDF

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Publication number
CN113289370A
CN113289370A CN202110665110.XA CN202110665110A CN113289370A CN 113289370 A CN113289370 A CN 113289370A CN 202110665110 A CN202110665110 A CN 202110665110A CN 113289370 A CN113289370 A CN 113289370A
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stirring
phenylalanine
box body
rotating shaft
continuous crystallization
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Chinese (zh)
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马云峰
马铭泽
杨静文
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Anhui Anlitai Biotechnology Co ltd
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Anhui Anlitai Biotechnology Co ltd
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    • 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
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/09—Stirrers characterised by the mounting of the stirrers with respect to the receptacle
    • B01F27/091—Stirrers characterised by the mounting of the stirrers with respect to the receptacle with elements co-operating with receptacle wall or bottom, e.g. for scraping the receptacle wall
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/116—Stirrers shaped as cylinders, balls or rollers
    • B01F27/1163—Rollers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/10—Maintenance of mixers
    • B01F35/12—Maintenance of mixers using mechanical means
    • B01F35/123—Maintenance of mixers using mechanical means using scrapers for cleaning mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/7173—Feed mechanisms characterised by the means for feeding the components to the mixer using gravity, e.g. from a hopper
    • B01F35/71731—Feed mechanisms characterised by the means for feeding the components to the mixer using gravity, e.g. from a hopper using a hopper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/7174—Feed mechanisms characterised by the means for feeding the components to the mixer using pistons, plungers or syringes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/75—Discharge mechanisms
    • B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
    • B01F35/75455—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle
    • B01F35/754551—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle using helical screws
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/95—Heating or cooling systems using heated or cooled stirrers
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38—Separation; Purification; Stabilisation; Use of additives
    • C07C227/40—Separation; Purification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38—Separation; Purification; Stabilisation; Use of additives
    • C07C227/40—Separation; Purification
    • C07C227/42—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F2035/99—Heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/2204—Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The continuous crystallization purification method of DL-phenylalanine comprises the following steps: heating the interior of the stirring box body to 70-80 ℃, adding water and a nonionic surfactant to dissolve crude DL-phenylalanine; heating to 10 ℃, and stirring for 30-40 minutes while heating by a stirring mechanism; adding ethanol into the stirring box body through the feeding part, and then cooling to the original dissolving temperature; discharging the crystal mush continuously through a discharging mechanism, and filtering and drying to obtain the purified DL-phenylalanine. The continuous crystallization purification method of DL-phenylalanine has the advantages of high efficiency during stirring and temperature rising, complete and thorough stirring, reduction of adhesion of DL-phenylalanine to the inner wall of the stirring box body, guarantee of more uniform particle size distribution of the purified DL-phenylalanine, and improvement of purification efficiency and quality.

Description

DL-phenylalanine continuous crystallization purification method
Technical Field
The invention belongs to the technical field of DL-phenylalanine treatment, and particularly relates to a continuous crystallization and purification method of high-purity DL-phenylalanine.
Background
DL-phenylalanine, also known as DL-alpha-amino-beta-phenylpropionic acid, has the chemical formula C9H11NO2DL-phenylalanine is one of essential amino acids in human body, and its main function is to ensure normal operation of central nervous system; in addition, it has effects in controlling depression and chronic disease symptoms, and diseases associated with central nervous system failure.
DL-phenylalanine is mainly used as biochemical reagent, medicine, feed and food additive, and nutritional supplement.
The chemical synthesis route in the prior DL-phenylalanine industrial production is mature, but the problems of low product purification efficiency and uneven particle size distribution still exist in the subsequent crystallization process; these problems limit the production and use of DL-phenylalanine, which cannot meet the market demand well, and have certain limitations.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a DL-phenylalanine continuous crystallization purification method, which has the following specific technical scheme:
the continuous crystallization purification method of DL-phenylalanine comprises the following steps:
heating the interior of the stirring box body to 70-80 ℃, adding water and a nonionic surfactant to dissolve crude DL-phenylalanine;
heating to 10 ℃, and stirring for 30-40 minutes while heating by a stirring mechanism;
adding ethanol into the stirring box body through the feeding part, and then cooling to the original dissolving temperature;
discharging the crystal mush continuously through a discharging mechanism, and filtering and drying to obtain the purified DL-phenylalanine.
Further, the heating up to 10 ℃ and the stirring up by the stirring mechanism for 30-40 minutes at the same time comprises the following steps:
the temperature in the stirring box body is raised by opening the first electric heating wire and the second electric heating wire;
meanwhile, the first motor is turned on, so that the first stirring piece and the second stirring piece of the spiral structure stir the interior of the stirring box body and scrape the inner wall.
Further, add ethanol to the agitator tank through the material loading spare, then cool to former dissolving temperature, include:
pouring ethanol into the blanking barrel, and pushing the push rod;
the ethanol enters the stirring box body through a discharge hole;
and communicating the stirring box body with refrigeration equipment, and cooling under the stirring effect.
Further, the crystal mush is continuously discharged through a discharging mechanism, and the purified glycine is obtained through filtering treatment, and the method comprises the following steps:
opening a second motor and a valve to enable the spiral piece to rotate to push out the crystal mush;
and filtering the crystal mush, and drying in hot air to obtain the purified DL-phenylalanine.
Further, the ratio of the water to the nonionic surfactant is 100:5, and at least 1000ml of water is required for dissolving per 100g of crude DL-phenylalanine.
Further, the ratio of the ethanol to the water is 30: 100, and slowly adding the ethanol into the stirring box body.
Further, the stirring mechanism comprises a first motor, a first rotating shaft, a transverse plate, a first stirring piece and a second stirring piece; first pivot is connected to the bottom of first motor, just the bottom mounting of first pivot has the diaphragm, just the bottom both sides of diaphragm are fixed with the first stirring piece and the second stirring piece that the structure is the same.
Further, the first stirring piece comprises a stirring roller, a first electric heating wire, a side scraping plate and a bottom scraping plate, the first electric heating wire is wound on the outer side of the stirring roller, and the stirring roller is of a spiral structure; a side scraper is fixed on the side part of the stirring roller, and a bottom scraper is fixed at the bottom end of the stirring roller; the side scraping plates and the bottom scraping plate adopt tooth-shaped structures; and the tooth-shaped structures of the side scraping plate and the bottom scraping plate in the first stirring piece and the second stirring piece are staggered with each other.
Further, the blanking mechanism comprises a valve, a blanking box body, a spiral piece, a second rotating shaft and a second motor, the blanking box body is communicated with a blanking port in the side part of the stirring box body, and the interior of the blanking box body is rotatably connected with the second rotating shaft; a spiral sheet is fixed on the outer side of the second rotating shaft, and the end part of the second rotating shaft is connected with a second motor; the bottom opening of unloading box, just the bottom opening part of unloading box is equipped with the valve.
Further, the feeding part comprises a push rod, a rubber plug, a feeding cylinder and a connector, the feeding cylinder is fixed at the top end of the stirring box body, and the rubber plug is connected to the inner part of the feeding cylinder in a sliding manner; a push rod is fixed at the top end of the rubber plug; the bottom end of the feeding barrel is connected with a connector through a pipeline, and the connector is fixed inside the stirring box body; the connector is rotationally connected to the outer side of the first rotating shaft, and the pipeline is communicated with the first rotating shaft through the connector; the first rotating shaft is of a hollow structure, and the bottom end of the first rotating shaft is communicated with the transverse plate; the transverse plate is of a hollow structure, and a discharge hole is formed in the bottom end of the transverse plate.
The invention has the beneficial effects that: the continuous crystallization purification method of DL-phenylalanine has the advantages of high efficiency during stirring and temperature rising, complete and thorough stirring, reduction of adhesion of DL-phenylalanine to the inner wall of the stirring box body, guarantee of more uniform particle size distribution of the purified DL-phenylalanine, and improvement of purification efficiency and quality.
Drawings
FIG. 1 is a schematic view showing the structure of a continuous crystallization purification apparatus for DL-phenylalanine according to the present invention;
shown in the figure: 1. stirring mechanism, 11, first motor, 12, first pivot, 13, diaphragm, 131, discharge opening, 14, first stirring piece, 141, stirring roller, 142, first electric heating wire, 143, side scraper blade, 144, end scraper blade, 15, second stirring piece, 2, second electric heating wire, 3, unloading mechanism, 31, valve, 32, unloading box, 33, flight, 34, second pivot, 35, second motor, 4, stirring box, 41, feed opening, 42, feeder hopper, 5, reinforced piece, 51, push rod, 52, rubber buffer, 53, feed cylinder, 54, the connecting head.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The continuous crystallization purification method of DL-phenylalanine comprises the following steps:
the method comprises the following steps: heating the interior of the stirring box body 4 to 70-80 ℃, and adding water and a nonionic surfactant to dissolve crude DL-phenylalanine;
specifically, the first electric heating wire 142 and the second electric heating wire 2 are opened to heat the inside of the stirring box body 4, and then water and a nonionic surfactant are added into the stirring box body 4 through the feed hopper 42 to dissolve crude DL-phenylalanine; wherein: the ratio of the water to the nonionic surfactant is 100:5, and at least 1000ml of water is needed for dissolving per 100g of crude DL-phenylalanine.
Step two: heating to 10 ℃, and stirring for 30-40 minutes while heating through the stirring mechanism 1;
specifically, the heating up to 10 ℃ and the stirring for 30-40 minutes while heating up by the stirring mechanism 1 include:
the temperature inside the agitation chamber 4 is raised by opening the first electric heating wire 142 and the second electric heating wire 2;
at the same time, the first motor 11 is turned on, so that the first stirring bar 14 and the second stirring bar 15 of the spiral structure stir the inside of the stirring box body 4 and scrape the inner wall.
Step three: adding ethanol into the stirring box body 4 through the feeding part 5, and then cooling to the original dissolving temperature;
specifically, add ethanol through the material loading spare in to agitator tank 4, then cool down to former dissolving temperature, include:
pouring ethanol into the blanking barrel 53, and pushing the push rod 51;
the ethanol enters the stirring box body 4 through a discharge hole 131;
the stirring box body 4 is communicated with refrigeration equipment, and is cooled under the stirring effect;
wherein the ratio of the ethanol to the water is 30: 100, and slowly adding the ethanol into the stirring box body;
the refrigerating equipment mainly comprises a compressor, an expansion valve, an evaporator, a condenser, accessories and pipelines; according to the working principle, the refrigeration device can be divided into a compression refrigeration device, an absorption refrigeration device, a steam injection refrigeration device, a heat pump refrigeration device, an electric heating refrigeration device and the like; the heat of the object and the surrounding is removed through the working cycle of the equipment, so that a certain low-temperature state is caused and maintained; the refrigerants used at present are mainly freon and ammonia, and freon is the most used particularly.
Step four: discharging crystal mush continuously through a discharging mechanism 3, and filtering and drying to obtain purified DL-phenylalanine.
Specifically, the continuous discharge of the crystal slurry through the discharging mechanism 3 and the filtration treatment to obtain the purified DL-phenylalanine comprise:
opening a second motor 35 and a valve 31 to enable the spiral piece 33 to rotate to push out the crystal mush;
and filtering the crystal mush, and drying in hot air to obtain the purified DL-phenylalanine.
Illustratively, 10000ml of water, 500ml of a nonionic surfactant, 1000g of crude DL-phenylalanine, and 3000ml of ethanol; the following operations are carried out:
the first electric heating wire 142 and the second electric heating wire 2 are opened to heat the stirring box body 4, and then water and a nonionic surfactant are added into the stirring box body 4 through the feed hopper 42 to dissolve crude DL-phenylalanine;
the temperature inside the stirring tank 4 is raised by 10 ℃ by opening the first electric heating wire 142 and the second electric heating wire 2;
meanwhile, the first motor 11 is turned on, so that the first stirring piece 14 and the second stirring piece 15 which are in a spiral structure stir the interior of the stirring box body 4 and scrape the inner wall;
then, pouring the ethanol into the blanking barrel 53 to push the push rod 51;
the ethanol enters the stirring box body 4 through a discharge hole 131;
the stirring box body 4 is communicated with refrigeration equipment, and is cooled under the stirring effect;
opening a second motor 35 and a valve 31 to enable the spiral piece 33 to rotate to push out the crystal mush;
and filtering the crystal mush, and drying in hot air to obtain the purified DL-phenylalanine.
The stirring mechanism 1 comprises a first motor 11, a first rotating shaft 12, a transverse plate 13, a first stirring piece 14 and a second stirring piece 15; first pivot 12 is connected to the bottom of first motor 11, just the bottom mounting of first pivot 12 has diaphragm 13, the bottom mounting of diaphragm 13 has the same first stirring piece 14 of structure and second stirring piece 15.
The first stirring member 14 comprises a stirring roller 141, a first electric heating wire 142, a side scraping plate 143 and a bottom scraping plate 144, the first electric heating wire 142 is wound on the outer side of the stirring roller 141, and the stirring roller 141 adopts a spiral structure; a side scraper 143 is fixed to the side of the stirring roller 141, and a bottom scraper 144 is fixed to the bottom end of the stirring roller 141; the side scrapers 142 and the bottom scrapers 144 adopt tooth-shaped structures; and the tooth-shaped structures of the side scraper 142 and the bottom scraper 144 in the first stirring part 14 and the second stirring part 15 are staggered with each other, so that the glycine is stirred more comprehensively, wall adhesion is avoided, and the grain size of the crystallized DL-phenylalanine is more average.
The blanking mechanism 3 comprises a valve 31, a blanking box body 32, a spiral sheet 33, a second rotating shaft 34 and a second motor 35, the blanking box body 32 is communicated with a blanking port 41 at the side part of the stirring box body 4, and the interior of the blanking box body 32 is rotatably connected with the second rotating shaft 34; a spiral sheet 33 is fixed on the outer side of the second rotating shaft 34, and the end part of the second rotating shaft 34 is connected with a second motor 35; the bottom opening of the blanking box body 32 is provided, the valve 31 is arranged at the bottom opening of the blanking box body 32, so that blanking is ensured to be uniform, the stirring box body 4 can be rotated if necessary, and the blanking is ensured to be comprehensive
The feeding part 5 comprises a push rod 51, a rubber plug 52, a feeding barrel 53 and a connector 54, the feeding barrel 53 is fixed at the top end of the stirring box body 4, and the rubber plug 52 is connected in the feeding barrel 53 in a sliding manner; a push rod 51 is fixed at the top end of the rubber plug 52; the bottom end of the charging barrel 53 is connected with a connector 54 through a pipeline, and the connector 54 is fixed in the stirring box body 4; the joint 54 is rotatably connected to the outer side of the first rotating shaft 12, and the pipeline is communicated with the first rotating shaft 12 through the joint 54; the first rotating shaft 12 is of a hollow structure, and the bottom end of the first rotating shaft 12 is communicated with a transverse plate 13; diaphragm 13 adopts hollow structure, just discharge hole 131 is seted up to the bottom of diaphragm 13, realizes from top to bottom carrying out the ethanol and adds, ensures more comprehensive with it mixes, can realize simultaneously adding in raw material when the stirring, improves material mixing rate.
Fig. 1 is a schematic overall structure diagram of an embodiment of the present invention, exemplarily, as shown in fig. 1, including a stirring box 4, where a stirring mechanism 1 is disposed inside the stirring box 4, and the stirring mechanism 1 includes a first motor 11, a first rotating shaft 12, a transverse plate 13, a first stirring member 14, and a second stirring member 15; the bottom end of the first motor 11 is connected with a first rotating shaft 12, a transverse plate 13 is fixed at the bottom end of the first rotating shaft 12, and a first stirring piece 14 and a second stirring piece 15 which are identical in structure are fixed at the bottom end of the transverse plate 13; the first stirring member 14 comprises a stirring roller 141, a first electric heating wire 142, a side scraping plate 143 and a bottom scraping plate 144, the first electric heating wire 142 is wound on the outer side of the stirring roller 141, and the stirring roller 141 adopts a spiral structure; a side scraper 143 is fixed on the side of the stirring roller 141, and the side scraper 143 contacts with the side of the inner wall of the stirring box body 4; a bottom scraper 144 is fixed at the bottom end of the stirring roller 141, and the bottom scraper 144 is contacted with the bottom end of the inner wall of the stirring box body 4; the side scrapers 143 and the bottom scrapers 144 adopt tooth-shaped structures; the first stirring piece 14 and the second stirring piece 15 are symmetrically distributed, and the tooth-shaped structures of the side scraper 143 and the bottom scraper 144 in the first stirring piece 14 and the tooth-shaped structures of the side scraper 143 and the bottom scraper 144 in the second stirring piece 15 are staggered with each other; the inner wall and the bottom wall of the stirring box body 4 are scraped comprehensively, so that more comprehensive stirring is ensured, and the wall sticking phenomenon is avoided; when stirring, the first motor 11 is turned on, and the first rotating shaft 12 is driven to rotate by the first motor 11; when rotating, the first stirring piece 14 and the second stirring piece 15 are driven to rotate around the first rotating shaft 12; the stirring roller 141 stirs the inside, and the side scraper 143 and the bottom scraper 144 scrape the inner wall of the stirring box 4; ensuring that the stirring is more uniform; a feed hopper 42 is arranged on one side of the top end of the stirring box body 4, and a feeding part 5 is arranged on the top end of the stirring box body 4;
the feeding part 5 comprises a push rod 51, a rubber plug 52, a feeding barrel 53 and a connector 54, the feeding barrel 53 is fixed at the top end of the stirring box body 4, and the rubber plug 52 is connected in the feeding barrel 53 in a sliding manner; a push rod 51 is fixed at the top end of the rubber plug 52; the bottom end of the charging barrel 53 is connected with a connector 54 through a pipeline, and the connector 54 is fixed in the stirring box body 4; the joint 54 is rotatably connected to the outer side of the first rotating shaft 12, and the pipeline is communicated with the first rotating shaft 12 through the joint 54; the first rotating shaft 12 is of a hollow structure, and the bottom end of the first rotating shaft 12 is communicated with a transverse plate 13; the transverse plate 13 is of a hollow structure, and the bottom end of the transverse plate 13 is provided with a discharging hole 131; when feeding, the rubber stopper 52 is drawn out, the material is placed in the charging barrel 53, then the rubber stopper 52 is installed, the rubber stopper 52 is pressed through the push rod 51, or other stepping pushing devices are connected, so that the material in the charging barrel 53 passes through the connecting head 54 and the first rotating shaft 12, enters the transverse plate 13, and is discharged into the stirring box body 4 through the discharging hole 131.
The blanking mechanism 3 comprises a valve 31, a blanking box body 32, a spiral sheet 33, a second rotating shaft 34 and a second motor 35, the blanking box body 32 is communicated with a blanking port 41 at the side part of the stirring box body 4, and the interior of the blanking box body 32 is rotatably connected with the second rotating shaft 34; a spiral sheet 33 is fixed on the outer side of the second rotating shaft 34, and the end part of the second rotating shaft 34 is connected with a second motor 35; the bottom end of the blanking box body 32 is provided with an opening, and the opening at the bottom end of the blanking box body 32 is provided with a valve 31; a second electric heating wire 2 is arranged on the inner wall of the stirring box body 4; the second motor 35 drives the spiral sheet 33 to rotate, so that the material in the stirring box body 4 can be pushed to discharge.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

  1. A method for purifying DL-phenylalanine by continuous crystallization, which is characterized in that: the method comprises the following steps:
    heating the interior of the stirring box body to 70-80 ℃, adding water and a nonionic surfactant to dissolve crude DL-phenylalanine;
    heating to 10 ℃, and stirring for 30-40 minutes while heating by a stirring mechanism;
    adding ethanol into the stirring box body through the feeding part, and then cooling to the original dissolving temperature;
    discharging the crystal mush continuously through a discharging mechanism, and filtering and drying to obtain the purified DL-phenylalanine.
  2. 2. The continuous crystallization purification method of DL-phenylalanine according to claim 1, characterized in that: the heating is carried out for 10 ℃, and the stirring is carried out for 30-40 minutes while the heating is carried out through a stirring mechanism, wherein the heating comprises the following steps:
    the temperature in the stirring box body is raised by opening the first electric heating wire and the second electric heating wire;
    meanwhile, the first motor is turned on, so that the first stirring piece and the second stirring piece of the spiral structure stir the interior of the stirring box body and scrape the inner wall.
  3. 3. The continuous crystallization purification method of DL-phenylalanine according to claim 1, characterized in that: add ethanol to the agitator tank in through the material loading spare, then cool down to former dissolving temperature, include:
    pouring ethanol into the blanking barrel, and pushing the push rod;
    the ethanol enters the stirring box body through a discharge hole;
    and communicating the stirring box body with refrigeration equipment, and cooling under the stirring effect.
  4. 4. The continuous crystallization purification method of DL-phenylalanine according to claim 1, characterized in that: the method for continuously discharging crystal mush through the discharging mechanism and obtaining purified DL-phenylalanine through filtering treatment comprises the following steps:
    opening a second motor and a valve to enable the spiral sheet to rotate to push out the crystal mush;
    and filtering the crystal mush, and drying in hot air to obtain the purified DL-phenylalanine.
  5. 5. The continuous crystallization purification method of DL-phenylalanine according to claim 1, characterized in that: the ratio of the water to the nonionic surfactant is 100:5, and at least 1000ml of water is needed for dissolving per 100g of crude DL-phenylalanine.
  6. 6. The continuous crystallization purification method of DL-phenylalanine according to claim 1, characterized in that: the ratio of the ethanol to the water is 30: 100, and slowly adding the ethanol into the stirring box body.
  7. 7. The continuous crystallization purification method of DL-phenylalanine according to any one of claims 1 to 6, characterized in that: the stirring mechanism comprises a first motor, a first rotating shaft, a transverse plate, a first stirring piece and a second stirring piece; first pivot is connected to the bottom of first motor, just the bottom mounting of first pivot has the diaphragm, just the bottom both sides of diaphragm are fixed with the first stirring piece and the second stirring piece that the structure is the same.
  8. 8. The continuous crystallization purification process of DL-phenylalanine according to claim 7, characterized in that: the first stirring piece comprises a stirring roller, a first electric heating wire, a side scraping plate and a bottom scraping plate,
    a first electric heating wire is wound on the outer side of the stirring roller, and the stirring roller is of a spiral structure;
    a side scraper is fixed on the side part of the stirring roller, and a bottom scraper is fixed at the bottom end of the stirring roller;
    the side scraping plates and the bottom scraping plate adopt tooth-shaped structures;
    and the tooth-shaped structures of the side scraping plate and the bottom scraping plate in the first stirring piece and the second stirring piece are staggered with each other.
  9. 9. The continuous crystallization purification process of DL-phenylalanine according to claim 8, characterized in that: the blanking mechanism comprises a valve, a blanking box body, a spiral piece, a second rotating shaft and a second motor, the blanking box body is communicated with a blanking port in the side part of the stirring box body, and the interior of the blanking box body is rotatably connected with the second rotating shaft; a spiral sheet is fixed on the outer side of the second rotating shaft, and the end part of the second rotating shaft is connected with a second motor; the bottom opening of unloading box, just the bottom opening part of unloading box is equipped with the valve.
  10. 10. The continuous crystallization purification process of DL-phenylalanine according to claim 9, characterized in that: the feeding part comprises a push rod, a rubber plug, a feeding barrel and a connector, the feeding barrel is fixed at the top end of the stirring box body, and the rubber plug is connected to the inner part of the feeding barrel in a sliding manner; a push rod is fixed at the top end of the rubber plug; the bottom end of the feeding barrel is connected with a connector through a pipeline, and the connector is fixed inside the stirring box body; the connector is rotationally connected to the outer side of the first rotating shaft, and the pipeline is communicated with the first rotating shaft through the connector; the first rotating shaft is of a hollow structure, and the bottom end of the first rotating shaft is communicated with the transverse plate; the transverse plate is of a hollow structure, and a discharge hole is formed in the bottom end of the transverse plate.
CN202110665110.XA 2021-06-16 2021-06-16 DL-phenylalanine continuous crystallization purification method Pending CN113289370A (en)

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CN210752388U (en) * 2019-07-11 2020-06-16 贵州永佳防水科技有限公司 High-efficient water proof coating apparatus for producing
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Application publication date: 20210824