CN114085768B - Purification device and purification method for producing psicose - Google Patents
Purification device and purification method for producing psicose Download PDFInfo
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- CN114085768B CN114085768B CN202111333423.1A CN202111333423A CN114085768B CN 114085768 B CN114085768 B CN 114085768B CN 202111333423 A CN202111333423 A CN 202111333423A CN 114085768 B CN114085768 B CN 114085768B
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M21/00—Bioreactors or fermenters specially adapted for specific uses
- C12M21/18—Apparatus specially designed for the use of free, immobilized or carrier-bound enzymes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/24—Preparation of compounds containing saccharide radicals produced by the action of an isomerase, e.g. fructose
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K3/00—Invert sugar; Separation of glucose or fructose from invert sugar
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to the technical field of psicose, in particular to a purifying device and a purifying method for producing psicose, comprising a purifying bin, wherein an inner barrel is detachably connected in the purifying bin, an exchange cavity is arranged between the purifying bin and the inner barrel, a cover plate matched with the exchange cavity is detachably connected at the top edge of the purifying bin, and a water inlet pipe and a water outlet pipe which penetrate through the cover plate and are communicated with the inside of the exchange cavity are symmetrically arranged at two sides of the top of the cover plate; the top of the purification bin is detachably connected with a top cover, one side of the top cover is communicated with a feed pipe, the other side of the top cover is communicated with an air outlet pipe, an electromagnetic area is arranged on the lower surface of the top cover, a plurality of magnetic attraction grooves are uniformly arranged in a matrix in the electromagnetic area, and crystal carriers are magnetically adsorbed in the magnetic attraction grooves; the invention can promote the crystallization speed and quality of crystals in the psicose solution with supersaturation, and is beneficial to improving the purification quality of psicose crystals.
Description
Technical Field
The invention relates to the technical field of psicose, in particular to a purifying device and a purifying method for producing psicose.
Background
Psicose belongs to hexose and ketose in classification, is epimer corresponding to the carbon number three of D-fructose, has special functions of regulating blood sugar and the like and is beneficial to human health, and is evaluated as the most potential sucrose substitute. The method mainly comprises the steps of performing cloning expression, separation and refining on enzyme by using an enzyme immobilization transformation method, and then performing transformation by using a proper carrier immobilization. The psicose solution obtained through conversion and sequential simulated mobile chromatography separation often needs to be crystallized and purified to obtain a psicose crystal product with the required particle size and purity.
Patent number CN201911015344.9 provides a crystallization process of psicose, which discloses that the preliminary crystallization and deep crystallization processes of psicose at different temperatures obtain the particle size and purity of psicose crystals; however, the manner and timing of adding the seed crystal were not examined. In order to increase the purity of crystals, it is often necessary to use an operation method in which seed crystals are added to a high-viscosity psicose solution in a metastable region. Therefore, the existing psicose purifying device needs to be improved, so that the crystal seed adding mode and adding time can be reasonably and effectively controlled, higher-purity psicose crystals can be obtained, the quality of products is improved, and the production requirement is met.
Disclosure of Invention
The invention aims to provide a purification device and a purification method for producing psicose, which solve the problems that the psicose purification device in the prior art is simple in design and cannot reasonably and effectively control the adding mode and the adding time of seed crystals so as to obtain higher-purity psicose crystals, improve the quality of products and meet the production requirement.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the purifying device for producing psicose comprises a purifying bin, wherein an inner barrel is detachably connected in the purifying bin, an exchange cavity is arranged between the purifying bin and the inner barrel, a cover plate matched with the exchange cavity is detachably connected at the top edge of the purifying bin, and a water inlet pipe and a water outlet pipe which penetrate through the cover plate and are communicated with the inside of the exchange cavity are symmetrically arranged at two sides of the top of the cover plate;
the top of the purification bin is detachably connected with a top cover, one side of the top cover is communicated with a feed pipe, the other side of the top cover is communicated with an air outlet pipe, an electromagnetic area is arranged on the lower surface of the top cover, a plurality of magnetic attraction grooves are uniformly arranged in a matrix in the electromagnetic area, and crystal carriers are magnetically adsorbed in the magnetic attraction grooves;
the crystal carrier comprises an upper counterweight part and a lower counterweight part which are made of ferromagnetic materials, wherein the lower counterweight part is connected with a lantern ring, and the lantern ring is connected with the upper counterweight part through a porous net;
the stirring mechanism comprises a sealing component penetrating through the inner barrel and the purification bin and a rotating shaft, wherein a plurality of groups of stirring blades made of magnetic materials are arranged on the rotating shaft, the blades of two adjacent groups of stirring blades are arranged in a staggered mode, the number of the stirring blades is equal to that of the crystal carriers, and when the stirring blades are located at the initial position, the blades of the stirring blades correspond to the crystal carriers one by one;
the bottom of one side of the purification bin is connected with a collection bin through a bottom plate, the top of the collection bin is provided with a condenser, a vacuum pump is arranged in the collection bin, and a weighing unit is arranged below the collection bin; the output end of the condenser is communicated with the inside of the collecting bin, and the input end of the condenser is communicated with the air outlet pipe through a conveying pipe;
in the process of introducing circulating hot water into the exchange cavity through the water inlet pipe and the water outlet pipe to evaporate the psicose in the inner barrel, simultaneously vacuumizing the inner barrel through the vacuum pump and the conveying pipe, condensing the evaporated substances through the condenser, and recycling the condensed substances into the collection bin; when the weight of the collecting bin measured by the weighing unit reaches a preset value, the control system controls the electromagnet in the electromagnetic area to be powered off, the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel, and then is magnetically adsorbed on the stirring blade, and the stirring blade drives the crystal carrier to rotate, so that psicose crystals in the crystal carrier penetrate through the porous net and are uniformly dispersed into the inner barrel.
The invention also provides a purification method of psicose, which adopts a purification device to purify the psicose and comprises the following steps:
s1, using crystalline glucose as a raw material, and converting the crystalline glucose by using isomerase to obtain fructose syrup;
s2, decoloring and ion-exchanging the fructose syrup, and separating the fructose syrup by using a high-efficiency simulated moving bed to obtain high fructose syrup with the fructose content more than 98%;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup through epimerase;
s5, separating the fructose and psicose mixed syrup through sequential simulated mobile chromatography to obtain a psicose solution with the purity of 98.5%;
s6, injecting the psicose solution into an inner barrel through a feed pipe, crystallizing and purifying to obtain psicose crystals and mother liquor;
s7, centrifugally separating the crystalline psicose and the mother liquor, and drying and screening psicose crystals to obtain psicose crystal products; the separated mother liquor is recycled.
Specifically, the step S6 specifically includes the following steps:
s601, injecting the psicose solution into an inner barrel through a feed pipe, starting a water inlet pipe and a water outlet pipe to introduce circulating hot water into the exchange cavity, heating the psicose solution in the inner barrel, and evaporating and crystallizing;
s602, starting a vacuum pump, vacuumizing the inner barrel, pumping the evaporated substances to a condenser through a conveying pipe and an air outlet pipe, condensing by the condenser to liquefy, and collecting the evaporated substances in a collecting bin;
s603, when the weighing unit detects that the weight of the collecting bin reaches a preset value, the control system controls the electromagnet in the electromagnetic area to be powered off, and the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel;
s604, magnetically adsorbing the crystal carrier separated from the electromagnetic area on a stirring blade, and driving the crystal carrier to rotate by the stirring blade, so that psicose crystals in the crystal carrier penetrate through a porous net and are uniformly dispersed into an inner barrel, and promoting the preliminary crystallization of psicose solution in the inner barrel;
s605, after the psicose solution is primarily crystallized, circulating cold water is introduced into the exchange cavity through the water inlet pipe and the water outlet pipe, and the psicose solution in the inner barrel is cooled; and (3) carrying out deep crystallization on the psicose solution subjected to preliminary crystallization in a vacuum environment until the crystallization work is completed.
The invention has at least the following beneficial effects:
1. according to the invention, when the psicose is purified by arranging the inner barrel, the exchange cavity, the condenser and the like, the psicose is added into the inner barrel through the feed pipe, the water inlet pipe and the water outlet pipe are opened to introduce circulating hot water into the exchange cavity, heat is transferred to the inner barrel, and the psicose solution in the inner barrel is heated and then enters an evaporation crystallization stage; according to the crystallization process of the psicose solution, circulating cold water is introduced into the exchange cavity through the water inlet pipe and the water outlet pipe, and the psicose solution in the inner barrel is cooled so as to carry out deep crystallization. In the process of evaporation and crystallization, the psicose solution heated evaporant enters a condenser through a conveying pipe, and enters a collecting bin for unified collection after being condensed and liquefied by the condenser. The device has reasonable structure, can heat or cool the inner barrel according to the crystallization process of the psicose so as to carry out evaporation crystallization and cooling deep crystallization, can control the vacuum degree in the inner barrel, promote the crystallization of crystals in the psicose solution with supersaturation degree, and improve the crystallization speed and quality of the psicose solution.
2. According to the invention, the crystal carrier is arranged and is matched with an electromagnetic area, stirring blades and the like to work together, so that in the process of adding the crystal seed, after the crystal seed carrier falls off from a magnetic absorption groove, the crystal seed carrier passes through the blade of the corresponding stirring blade, and finally is magnetically adsorbed on the blade of the corresponding stirring blade, so that the follow-up synchronous rotation of the corresponding blade is ensured, and in the process of rotating along with the blade, the crystal seed of the crystal seed in the crystal seed carrier can pass through the mesh of a porous net and uniformly disperse into the crystal seed of the crystal seed.
3. According to the invention, the collecting bin, the condenser, the weighing unit, the electromagnetic area, the crystal carrier and the stirring blade are cooperated to work, on one hand, the weight of an evaporating substance in the evaporating crystallization stage is measured through the condenser and the weighing unit, the evaporating substance is recycled, and meanwhile, the condition that the psicose solution reaches the metastable area of the supersaturated solution is used as a condition for triggering the electromagnetic area to release the crystal carrier is used; after the crystal carrier is separated from the electromagnetic area, the crystal carrier is further magnetically adsorbed on the blades of the corresponding stirring blades, and in the rotation process of the blades of the stirring blades, the psicose crystal seeds in the crystal seed carrier can pass through meshes of a porous net and are uniformly dispersed into the psicose solution under the action of centrifugal force generated by rotation of the blades and resistance impact of the psicose solution, so that the multipoint and dynamic addition of the psicose crystal seeds are realized, the distribution uniformity of the psicose crystal seeds in the solution is further greatly improved, and the subsequent crystallization effect is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic view of the structure of the top cover and the purifying bin of the present invention;
FIG. 3 is a schematic diagram of the purification bin and exchange chamber structure of the present invention;
FIG. 4 is a schematic diagram of a driving portion according to the present invention;
FIG. 5 is a schematic view of the structure of the electromagnetic area and the magnetic attraction groove on the top cover of the invention;
FIG. 6 is a schematic diagram of the structure of a crystalline support according to the present invention;
FIG. 7 is a schematic view of a stirring vane and shaft structure according to the present invention;
FIG. 8 is a schematic top view of the crystal carrier of the present invention magnetically adsorbed on the stirring blade;
FIG. 9 shows a flow chart of the psicose purification process of the present invention.
In the figure: 1. a driving section; 101. docking the screw; 102. a mounting plate; 103. a motor; 104. a fixed block; 105. a rotating shaft; 106. a fixed screw; 107. a butt-joint nut; 108. a butt joint block; 2. a crystal carrier; 201. an upper counterweight portion; 202. a lower counterweight portion; 203. a collar; 204. a porous web; 3. a carrying plate; 4. purifying bin; 5. a delivery tube; 6. a condenser; 7. a jacket clamp; 8. a support frame; 9. a collecting bin; 10. a feed pipe; 11. stirring blades; 12. an air outlet pipe; 13. a top cover; 14. an exchange chamber; 15. a water inlet pipe; 16. an inner barrel; 17. a cover plate; 18. a water outlet pipe; 19. an electromagnetic region; 20. a magnetic attraction groove.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1 to 4, a purifying device for producing psicose comprises a purifying bin 4, wherein an inner barrel 16 is detachably connected to the inside of the purifying bin 4, and the inner barrel 16 is used for purifying psicose solution crystal; an exchange cavity 14 is arranged between the purification bin 4 and the inner barrel 16, circulating cold water or hot water is introduced into the exchange cavity 14, hot water is introduced into the exchange cavity for heating when the psicose solution is evaporated and crystallized so as to evaporate, and then cold water is introduced into the exchange cavity for cooling so as to perform deep crystallization. The top edge of the purifying bin 4 is detachably connected with a cover plate 17 matched with the exchange cavity 14, and a water inlet pipe 15 and a water outlet pipe 18 which penetrate through the cover plate 17 and are communicated with the inside of the exchange cavity 14 are symmetrically arranged on two sides of the top of the cover plate 17; hot water or cold water can be introduced through the water inlet pipe 15 and the water outlet pipe 18 according to the progress of the psicose crystallization, so that heat exchange is realized, and the evaporation crystallization and the cooling crystallization are correspondingly carried out.
The top of purification storehouse 4 can be dismantled and be connected with top cap 13, and the top of top cap 13 one side intercommunication has inlet pipe 10, and the opposite side intercommunication has outlet duct 12. The feed tube 10 is used to add the psicose solution into the inner barrel 16.
The stirring mechanism is arranged at the center of the bottom of the inner cavity of the inner barrel 16 and comprises a sealing component and a rotating shaft 105 penetrating through the inner barrel 16 and the purifying bin 4, the rotating shaft 105 is connected with the driving part 1, and the stirring mechanism can be driven to rotate through the driving part 1 and the rotating shaft 105 so as to stir the psicose solution in the purifying bin 4, ensure that the psicose solution in the purifying bin 4 is heated uniformly, facilitate crystallization of psicose crystals and improve crystallization quality.
The bottom of one side of the purification bin 4 is connected with a collection bin 9 through a bottom plate, and a vacuum pump is arranged in the collection bin 9, so that on one hand, the vacuum pump can vacuumize the upper part in the inner barrel 16 and promote crystallization of crystals in the supersaturated psicose solution; on the other hand, in the evaporation crystallization stage, the evaporated substance of the psicose solution can be sucked into the collecting bin 9.
The top of collection storehouse 9 is provided with condenser 6, and the output of condenser 6 is linked together with the inside of collection storehouse 9, and the input of condenser 6 communicates with outlet duct 12 through conveyer pipe 5. In the process of evaporating and crystallizing the psicose solution in the purifying bin 4, the evaporated substance is pumped to the condenser 6 through the vacuum pump, the conveying pipe 5 and the air outlet pipe 12, is liquefied through the condensation action of the condenser 6, and finally is collected in the collecting bin 9 to be reused.
In the process of evaporating and crystallizing the psicose solution and cooling the psicose solution in a vacuum environment to separate and obtain psicose crystals, the temperature and the vacuum degree during crystallization are the most critical factors, and too high or too low temperature and too high vacuum degree can lead the psicose solution to enter a high-supersaturation state, so that the granularity of crystal particles becomes small, and the yield and the purity of the crystals are affected; too high a temperature can cause allose denaturation and also affect purity; therefore, in the process of concentrating, cooling and separating the psicose for crystallization, two external conditions of temperature and vacuum degree are strictly controlled to ensure the crystallization purity of the psicose; in the device, when the psicose needs to be crystallized and purified through the arrangement of the exchange cavity 14 and the inner barrel 16, the psicose is added into the inner barrel 16 through the feed pipe 10, the water inlet pipe 15 and the water outlet pipe 18 are opened to introduce circulating hot water into the exchange cavity 14, heat is transferred to the inner barrel 16, and the psicose solution in the inner barrel 16 is heated and enters an evaporation and crystallization stage; according to the progress of the crystallization of the psicose solution, circulating cold water is introduced into the exchange chamber 14 through the water inlet pipe 15 and the water outlet pipe 18, and the psicose solution in the inner barrel 16 is cooled to perform deep crystallization.
In the process of evaporation and crystallization, the psicose solution heated evaporant enters a condenser 6 through a conveying pipe 5, is condensed and liquefied by the condenser, and then enters a collecting bin 9 for unified collection. The device has reasonable structure, can heat or cool the inner barrel 16 according to the crystallization process of the psicose so as to carry out evaporative crystallization and cooling deep crystallization, can control the vacuum degree in the inner barrel 16, promote the crystallization of crystals in the psicose solution with supersaturation degree, and improve the crystallization speed and quality of the psicose solution.
Further, the bottom of the inner barrel 16 is fixedly connected with the bottom of the inner cavity of the purifying bin 4 through bolts, the top cover 13 is connected with the top of the purifying bin 4 in a sealing mode, and specifically, through the arrangement of the inner barrel 16, the inside impurities can be cleaned comprehensively.
Further, the outer lane of condenser 6 has cup jointed the cover clamp 7, and the equal fixedly connected with of both sides of cover clamp 7 is with bottom plate bolt fixed connection's support frame 8, specifically, through the setting of support frame 8, has guaranteed the installation stability of condenser 6.
Further, the purification storehouse 4 below is equipped with loading board 3, and the bottom of loading board 3 is provided with drive division 1, and drive division 1 includes the motor 103 of installing in loading board 3 bottom through mounting panel 102, and the output shaft of motor 103 is connected with the tip transmission of pivot 105, specifically, through the setting of motor 103, has improved the convenience of rotating pivot 105.
Further, the bottom both sides of mounting panel 102 all are provided with the dead screw 106 that one end runs through mounting panel 102, the one end bolt fixedly connected with of dead screw 106 and loading board 3 bottom fixed connection's fixed block 104, the other end fixedly connected with butt joint piece 108, the bottom level of mounting panel 102 is provided with butt joint screw 101, two butt joint piece 108 threaded connection has butt joint nut 107 are run through to the one end of butt joint screw 101, specifically, through the setting of mounting panel 102, be convenient for carry out the dismouting to motor 103, the later maintenance transportation of being convenient for.
To sum up: when the psicose needs to be purified, the psicose is added into the inner barrel 16 through the feed pipe 10, the water inlet pipe 15 and the water outlet pipe 18 are opened to introduce circulating hot water into the exchange cavity 14, heat is transferred to the inner barrel 16, and the psicose solution in the inner barrel 16 is heated and then enters an evaporation crystallization stage; according to the progress of the crystallization of the psicose solution, circulating cold water is introduced into the exchange chamber 14 through the water inlet pipe 15 and the water outlet pipe 18, and the psicose solution in the inner barrel 16 is cooled to perform deep crystallization. In the process of evaporation and crystallization, the psicose solution heated evaporant enters a condenser 6 through a conveying pipe 5, is condensed and liquefied by the condenser, and then enters a collecting bin 9 for unified collection. The device has reasonable structure, can heat or cool the inner barrel 16 according to the crystallization process of the psicose so as to carry out evaporative crystallization and cooling deep crystallization, can control the vacuum degree in the inner barrel 16, promote the crystallization of crystals in the psicose solution with supersaturation degree, and improve the crystallization speed and quality of the psicose solution.
Example 2
In order to improve the crystallization rate and ensure the product quality, seed crystals are often required to be added in the crystallization process of the psicose solution. For psicose solution with higher solution viscosity, crystal nucleus generation is difficult, and when crystallization is carried out under higher supersaturation degree, the crystal nucleus formation rate is higher, so that the polycrystalline phenomenon is easy to occur, and the product quality is not easy to control. Therefore, a high viscosity psicose solution must be subjected to an operation method of adding seed crystals in the metastable zone. Thus, the timing of seeding must be well known, the seeding should be performed at the appropriate temperature at which the solution enters the metastable zone, and the seeding should be gently agitated to uniformly disperse the seeds in the solution. Therefore, the device is further improved for achieving the aim.
As shown in fig. 5-8, an electromagnetic area 19 is arranged on the lower surface of the top cover 13, a plurality of magnetic attraction grooves 20 are uniformly arranged in the electromagnetic area 19 in a matrix manner, and crystal carriers 2 are magnetically attracted in the magnetic attraction grooves 20; the crystal carrier 2 comprises an upper counterweight part 201 and a lower counterweight part 202 which are made of ferromagnetic materials, wherein a lantern ring 203 is connected to the lower counterweight part 202, and the lantern ring 203 is connected with the upper counterweight part 201 through a porous net 204; before adding the seed crystal, the psicose seed crystal can be poured into the lantern ring 203 through the porous net 204, then the electromagnetic area 19 is controlled to be electrified through the control system to generate magnetism, the magnetism is magnetized to the magnetism sucking groove 20, and then the crystal carrier 2 is magnetically adsorbed in the magnetism sucking groove 20 through the upper counterweight part 201, so that preparation is made for adding the psicose seed crystal in advance. The arrangement of the upper weight portion 201 and the lower weight portion 202 can increase the weight of the crystal carrier 2, so as to ensure that the crystal carrier 2 can smoothly pass through the psicose solution with higher viscosity and be magnetically adsorbed on the corresponding blade in the psicose solution entering the inner barrel 16.
Specifically, the pore size of the porous mesh 204 is larger than the particle size of the psicose crystals to ensure that the psicose seeds can be uniformly dispersed into the psicose solution through the mesh of the porous mesh 204 when the seeds are added later.
Specifically, the stirring blades 11 made of multiple groups of magnetic materials are arranged on the rotating shaft 105, the blades of two adjacent stirring blades 11 are arranged in a staggered manner, the number of the blades of the stirring blades 11 is equal to that of the crystal carriers 2, when the stirring blades 11 are positioned at the initial position, the blades of the stirring blades 11 are in one-to-one correspondence with the crystal carriers 2, so that in the process of adding seed crystals, after the seed crystal carriers 2 fall off from the magnetic suction grooves 20, the seed crystal carriers 2 pass through the psicose solution and can fall onto the corresponding blades of the stirring blades 11, and finally the seed crystal carriers pass through the psicose solution and are magnetically adsorbed onto the corresponding blades of the stirring blades 11, so that the follow-up synchronous rotation of the corresponding blades is ensured.
Further, the motor 103 adopts a servo motor to ensure that the motor 103 can be accurately controlled to reach an initial position every time when stopping, and the blades on the stirring blades 11 can be in one-to-one correspondence with the corresponding crystal carriers 2 at the initial position, so that the crystal carriers 2 can be magnetically adsorbed on the blades of the corresponding stirring blades 11 after falling off from the electromagnetic area 19.
Specifically, the stirring blades 11 are provided with two groups, the number of blades on each group of stirring blades 11 is four, and the total number of blades of the stirring blades 11 is equal to the total number of the crystal carriers 2, so that the crystal carriers 2 can follow the rotation process of the blades after being magnetically adsorbed on the blades, the psicose seeds in the seed crystal carriers 2 can pass through meshes of the porous net 204 under the centrifugal force generated by rotation of the blades and the resistance impact effect of the psicose solution, and are uniformly dispersed into the psicose solution, so that the multipoint and dynamic addition of the psicose seeds is realized, the distribution uniformity of the psicose seeds in the solution is further greatly improved, and the subsequent crystallization effect is improved.
A weighing unit is arranged below the collecting bin 9; the weighing unit is used for weighing the added weight of the collecting bin 9; by setting the preset value of the weighing unit in the control system, when the weighing unit measures that the weight of the collecting bin 9 reaches the preset value, the psicose solution in the inner barrel 16 reaches the metastable zone of the supersaturated solution. Since the psicose solution just added into the purification bin 4 is an unsaturated solution, in the evaporation crystallization stage, a saturated solution is gradually formed along with the evaporation of the solution and enters the metastable zone. The evaporated substances are filled into a condenser 6 through a vacuum pump, a conveying pipe 5 and an air outlet pipe 12 to be condensed and liquefied, and then are collected in a collecting bin 9; the weight of the evaporating substances in the collecting bin 9 is calculated through the weighing unit, whether the psicose solution forms a saturated solution or not and enters a metastable zone (namely, the solution with a certain concentration can be understood, the amount of the solvent evaporated when the solution reaches the saturated concentration through heating evaporation can be calculated and measured), and the weight increment of the collecting bin 9 is calculated through the weighing unit to set a preset value so as to ensure that the time for adding the psicose seed crystal is controlled, namely, when the weight of the collecting bin 9 reaches the preset value measured by the weighing unit, the psicose solution in the purifying bin 4 reaches the metastable zone of the supersaturated solution, and the seed crystal is added at the moment, so that the crystallization rate can be improved and the quality of a crystallized product can be ensured.
By improving related devices, in the process of introducing circulating hot water into the exchange cavity 14 through the water inlet pipe 15 and the water outlet pipe 18 to evaporate psicose in the inner barrel 16, simultaneously vacuumizing the inner barrel 16 through the vacuum pump and the conveying pipe 5, condensing the evaporated substances through the condenser 6 and recycling the condensed substances into the collection bin 9; when the weighing unit measures that the weight of the collecting bin 9 reaches a preset value, the control system controls the electromagnet in the electromagnetic area 19 to be powered off, the crystal carrier 2 magnetically adsorbed by the magnetic attraction groove 20 falls off and descends into the inner barrel 16, the crystal carrier 2 passes through the psicose solution and is magnetically adsorbed on the stirring blade 11, and the stirring blade 11 drives the crystal carrier 2 to rotate, so that psicose crystals in the crystal carrier 2 pass through the porous net 204 and are uniformly dispersed into the inner barrel 16.
In summary, the collecting bin 9, the condenser 6, the weighing unit, the electromagnetic area 19, the crystal carrier 2 and the stirring blade 11 cooperate, on one hand, the weight of the evaporated substances in the evaporation crystallization stage is measured through the condenser and the weighing unit, and the evaporated substances are recycled and reused, and the conditions for judging that the psicose solution reaches the metastable area of the supersaturated solution and triggering the electromagnetic area 19 to release the crystal carrier 2 are used; after the crystal carrier 2 is separated from the electromagnetic region, the crystal carrier is further magnetically adsorbed on the blades of the corresponding stirring blades 11, and in the rotation process of the blades of the stirring blades 11, the psicose crystal seeds in the crystal carrier 2 can pass through the meshes of the porous net 204 and are uniformly dispersed into the psicose solution under the action of centrifugal force generated by rotation of the blades and resistance impact of the psicose solution, so that the multipoint and dynamic addition of the psicose crystal seeds is realized, the distribution uniformity of the psicose crystal seeds in the solution is further greatly improved, and the subsequent crystallization effect is improved.
Example 3
The invention also provides a purification method of psicose, which adopts a purification device to purify psicose, as shown in figure 9, and comprises the following steps:
s1, using crystalline glucose as a raw material, and converting the crystalline glucose by using isomerase to obtain fructose syrup;
s2, decoloring and ion-exchanging the fructose syrup, and separating the fructose syrup by using a high-efficiency simulated moving bed to obtain high fructose syrup with the fructose content more than 98%;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup through epimerase;
s5, separating the fructose and psicose mixed syrup through sequential simulated mobile chromatography to obtain a psicose solution with the purity of 98.5%;
s6, injecting the psicose solution into an inner barrel 16 through a feed pipe 10, crystallizing and purifying to obtain psicose crystals and mother liquor;
s7, centrifugally separating the crystalline psicose and the mother liquor, and drying and screening psicose crystals to obtain psicose crystal products; the separated mother liquor is recycled.
The step S6 specifically comprises the following steps:
s601, injecting the psicose solution into an inner barrel 16 through a feed pipe 10, opening a water inlet pipe 15 and a water outlet pipe 18, introducing circulating hot water into the exchange cavity 14, heating the psicose solution in the inner barrel 16, and performing evaporative crystallization;
s602, starting a vacuum pump, vacuumizing the inner barrel 16, pumping the evaporated substances to the condenser 6 through the conveying pipe 5 and the air outlet pipe 12, condensing by the condenser 6 to liquefy, and collecting the evaporated substances in the collecting bin 9;
s603, when the weighing unit measures that the weight of the collecting bin 9 reaches a preset value, the control system controls the electromagnet in the electromagnetic area 19 to be powered off, and the crystal carrier 2 magnetically adsorbed by the electromagnetic area 19 falls off and descends into the inner barrel 16;
s604, magnetically adsorbing the crystal carrier 2 separated from the electromagnetic area 19 on a stirring blade 11, and driving the crystal carrier 2 to rotate by the stirring blade 11, so that psicose crystals in the crystal carrier 2 pass through a porous net 204 and are uniformly dispersed into an inner barrel 16, and promoting the preliminary crystallization of psicose solution in the inner barrel 16;
s605, after the psicose solution is primarily crystallized, circulating cold water is introduced into the exchange cavity 14 through the water inlet pipe 15 and the water outlet pipe 18, the psicose solution in the inner barrel 16 is cooled, and the primarily crystallized psicose solution is deeply crystallized in a vacuum environment until the crystallization work is completed.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The purifying device for producing psicose comprises a purifying bin, and is characterized in that an inner barrel is detachably connected in the purifying bin, an exchange cavity is arranged between the purifying bin and the inner barrel, a cover plate matched with the exchange cavity is detachably connected at the edge of the top of the purifying bin, and a water inlet pipe and a water outlet pipe which penetrate through the cover plate and are communicated with the inside of the exchange cavity are symmetrically arranged at two sides of the top of the cover plate;
the top of the purification bin is detachably connected with a top cover, one side of the top cover is communicated with a feed pipe, the other side of the top cover is communicated with an air outlet pipe, an electromagnetic area is arranged on the lower surface of the top cover, a plurality of magnetic attraction grooves are uniformly arranged in a matrix in the electromagnetic area, and crystal carriers are magnetically adsorbed in the magnetic attraction grooves;
the crystal carrier comprises an upper counterweight part and a lower counterweight part which are made of ferromagnetic materials, wherein the lower counterweight part is connected with a lantern ring, and the lantern ring is connected with the upper counterweight part through a porous net;
the stirring mechanism comprises a sealing component penetrating through the inner barrel and the purification bin and a rotating shaft, wherein a plurality of groups of stirring blades made of magnetic materials are arranged on the rotating shaft, the blades of two adjacent groups of stirring blades are arranged in a staggered mode, the number of the stirring blades is equal to that of the crystal carriers, and when the stirring blades are located at the initial position, the blades of the stirring blades correspond to the crystal carriers one by one;
the bottom of one side of the purification bin is connected with a collection bin through a bottom plate, the top of the collection bin is provided with a condenser, a vacuum pump is arranged in the collection bin, and a weighing unit is arranged below the collection bin; the output end of the condenser is communicated with the inside of the collecting bin, and the input end of the condenser is communicated with the air outlet pipe through a conveying pipe;
in the process of introducing circulating hot water into the exchange cavity through the water inlet pipe and the water outlet pipe to evaporate the psicose in the inner barrel, simultaneously vacuumizing the inner barrel through the vacuum pump and the conveying pipe, condensing the evaporated substances through the condenser, and recycling the condensed substances into the collection bin; when the weight of the collecting bin measured by the weighing unit reaches a preset value, the control system controls the electromagnet in the electromagnetic area to be powered off, the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel, and then is magnetically adsorbed on the stirring blade, and the stirring blade drives the crystal carrier to rotate, so that psicose crystals in the crystal carrier penetrate through the porous net and are uniformly dispersed into the inner barrel;
when the weight of the collecting bin measured by the weighing unit reaches a preset value, the psicose solution in the inner barrel reaches a metastable zone of supersaturated solution.
2. A purification apparatus for producing psicose according to claim 1, wherein the stirring blades are provided in two groups, the number of blades on each group of stirring blades is four, and the total number of blades of stirring blades is equal to the total number of the crystal carriers.
3. A purification device for the production of psicose according to claim 1, characterized in that the pore size of the porous mesh is larger than the particle size of the psicose crystals.
4. The purifying device for producing psicose according to claim 1, wherein the bottom of the inner barrel is fixedly connected with a bottom bolt of an inner cavity of the purifying bin, and the top cover is hermetically connected with the top of the purifying bin.
5. The purifying device for producing psicose according to claim 1, wherein the outer ring of the condenser is sleeved with a jacket clamp, and two sides of the jacket clamp are fixedly connected with a supporting frame fixedly connected with a bottom plate bolt.
6. The purifying device for producing psicose according to claim 1, wherein a bearing plate is arranged below the purifying bin, a driving part is arranged at the bottom of the bearing plate, the driving part comprises a motor arranged at the bottom of the bearing plate through a mounting plate, and an output shaft of the motor is in transmission connection with the end part of the rotating shaft.
7. The purifying device for producing psicose according to claim 6, wherein two sides of the bottom of the mounting plate are provided with fixing screws, one ends of the fixing screws penetrate through the mounting plate, one end of each fixing screw is fixedly connected with a fixing block fixedly connected with the bottom of the bearing plate through bolts, the other end of each fixing screw is fixedly connected with a butt joint block, the bottom of the mounting plate is horizontally provided with a butt joint screw, and one ends of the butt joint screws penetrate through the two butt joint blocks and are in threaded connection with butt joint nuts.
8. A purification method of psicose using the purification apparatus according to any one of claims 1 to 7, characterized by comprising the steps of:
s1, using crystalline glucose as a raw material, and converting the crystalline glucose by using isomerase to obtain fructose syrup;
s2, decoloring and ion-exchanging the fructose syrup, and separating the fructose syrup by using a high-efficiency simulated moving bed to obtain high fructose syrup with the fructose content more than 98%;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup through epimerase;
s5, separating the fructose and psicose mixed syrup through sequential simulated mobile chromatography to obtain a psicose solution with the purity of 98.5%;
s6, injecting the psicose solution into an inner barrel through a feed pipe, crystallizing and purifying to obtain psicose crystals and mother liquor;
s7, centrifugally separating the crystalline psicose and the mother liquor, and drying and screening psicose crystals to obtain psicose crystal products; the separated mother liquor is recycled.
9. The method for purifying psicose according to claim 8, wherein the step S6 specifically comprises the steps of:
s601, injecting the psicose solution into an inner barrel through a feed pipe, starting a water inlet pipe and a water outlet pipe to introduce circulating hot water into the exchange cavity, heating the psicose solution in the inner barrel, and evaporating and crystallizing;
s602, starting a vacuum pump, vacuumizing the inner barrel, pumping the evaporated substances to a condenser through a conveying pipe and an air outlet pipe, condensing by the condenser to liquefy, and collecting the evaporated substances in a collecting bin;
s603, when the weighing unit detects that the weight of the collecting bin reaches a preset value, the control system controls the electromagnet in the electromagnetic area to be powered off, and the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel;
s604, magnetically adsorbing the crystal carrier separated from the electromagnetic area on a stirring blade, and driving the crystal carrier to rotate by the stirring blade, so that psicose crystals in the crystal carrier penetrate through a porous net and are uniformly dispersed into an inner barrel, and promoting the preliminary crystallization of psicose solution in the inner barrel;
s605, after the psicose solution is primarily crystallized, circulating cold water is introduced into the exchange cavity through the water inlet pipe and the water outlet pipe, and the psicose solution in the inner barrel is cooled; and (3) carrying out deep crystallization on the psicose solution subjected to preliminary crystallization in a vacuum environment until the crystallization work is completed.
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| US10808002B2 (en) * | 2014-10-20 | 2020-10-20 | Cj Cheiljedang Corporation | Method for preparing D-psicose crystal |
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