CN114085768A - Purification device and purification method for producing psicose - Google Patents

Purification device and purification method for producing psicose Download PDF

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CN114085768A
CN114085768A CN202111333423.1A CN202111333423A CN114085768A CN 114085768 A CN114085768 A CN 114085768A CN 202111333423 A CN202111333423 A CN 202111333423A CN 114085768 A CN114085768 A CN 114085768A
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psicose
inner barrel
purification
allulose
bin
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CN114085768B (en
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冯军伟
董必辉
周志强
刘世欣
段兰兰
闫佳佳
和利辉
常瑞波
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Henan Feitian Agricultural Development Co ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • C13K3/00Invert sugar; Separation of glucose or fructose from invert sugar
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Abstract

The invention relates to the technical field of psicose, in particular to a purification device and a purification method for producing psicose, which comprises a purification bin, wherein the interior of the purification bin is detachably connected with an inner barrel, an exchange cavity is arranged between the purification bin and the inner barrel, the edge of the top of the purification bin is detachably connected with a cover plate matched with the exchange cavity, and water inlet pipes and water outlet pipes which penetrate through the cover plate and are communicated with the interior of the exchange cavity are symmetrically arranged on 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 feeding 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 absorption grooves are uniformly arranged in a matrix manner in the electromagnetic area, and crystal carriers are magnetically absorbed in the magnetic absorption grooves; the method can promote the crystallization speed and quality of the crystals in the supersaturated allulose solution, and is favorable for improving the purification quality of allulose crystals.

Description

Purification device and purification method for producing psicose
Technical Field
The invention relates to the technical field of psicose, in particular to a purification device and a purification method for producing psicose.
Background
The psicose belongs to hexose and ketose in classification, is an epimer corresponding to the carbon at the third position of D-fructose, has special functions of regulating blood sugar and the like beneficial to human health, and is evaluated as the most potential sucrose substitute. It is prepared mainly by enzyme immobilization conversion method, i.e. cloning, expressing, separating and refining enzyme, then carrying out conversion by proper carrier immobilization. The psicose solution obtained through conversion and sequential simulated moving chromatography separation usually needs crystallization and purification to obtain the psicose crystal product with required particle size and purity.
Patent No. CN201911015344.9 provides a process for crystallizing psicose, which discloses that psicose is subjected to preliminary crystallization and deep crystallization at different temperatures to obtain the particle size and purity of psicose crystals; however, the method and timing of seed crystal addition were not investigated. In order to improve the purity of the crystals, the operation of adding seed crystals in a metastable zone is required to be adopted in the allulose solution with high viscosity. Therefore, the existing allulose purification device needs to be improved, so that the seed crystal adding mode and adding time are reasonably and effectively controlled, allulose crystals with higher purity are 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, and solves the problems that in the prior art, the design of the psicose purification device is simple, and the addition mode and the addition time of a seed crystal cannot be reasonably and effectively controlled to obtain a high-purity psicose crystal, improve the quality of a product and meet the production requirement.
In order to achieve the purpose, the invention adopts the following technical scheme:
a purification device for producing psicose comprises a purification bin, wherein an inner barrel is detachably connected inside the purification bin, an exchange cavity is arranged between the purification bin and the inner barrel, a cover plate matched with the exchange cavity is detachably connected to the edge of the top of the purification 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 installed on 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 feeding 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 absorption grooves are uniformly arranged in a matrix manner in the electromagnetic area, and crystal carriers are magnetically absorbed in the magnetic absorption grooves;
the crystal carrier comprises an upper counterweight part and a lower counterweight part which are made of ferromagnetic materials, 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;
a stirring mechanism is arranged at the center of the bottom of the inner cavity of the inner barrel and comprises a sealing assembly and a rotating shaft, the sealing assembly penetrates through the inner barrel and the purification bin, a plurality of groups of magnetic stirring blades are arranged on the rotating shaft, blades of two adjacent groups of stirring blades are arranged in a staggered mode, the number of the blades 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 interior 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 allulose in the inner barrel, simultaneously, the inner barrel is vacuumized through the vacuum pump and the conveying pipe, and evaporated substances are condensed by the condenser and then are recovered into the collection bin; when the weighing unit records 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, the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel, then the crystal carrier is magnetically adsorbed on the stirring blade, and the stirring blade drives the crystal carrier to rotate, so that the 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 the psicose, which adopts a purification device to purify the psicose and comprises the following steps:
s1, adopting crystalline glucose as a raw material, and converting the crystalline glucose by isomerase to obtain high fructose syrup;
s2, after the high fructose corn syrup is decolorized and ion-exchanged, separating the high fructose corn syrup by a high-efficiency simulated moving bed to obtain high fructose syrup with fructose content more than 98 percent;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain a fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup by using epimerase;
s5, separating the fructose and psicose mixed syrup by 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 crystallized allulose from the mother liquor, drying and screening allulose crystals to obtain allulose 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, opening a water inlet pipe and a water outlet pipe to introduce circulating hot water into an exchange cavity, heating the psicose solution in the inner barrel, and carrying out evaporative crystallization;
s602, starting a vacuum pump, vacuumizing the inner barrel, pumping evaporated substances to a condenser through a conveying pipe and an air outlet pipe, condensing and liquefying the evaporated substances through the condenser, and collecting the condensed substances into a collection 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, adsorbing the crystal carrier magnetic separated from the electromagnetic region on a stirring blade, and driving the crystal carrier to rotate by the stirring blade to enable the allulose crystals in the crystal carrier to penetrate through a porous net and be uniformly dispersed into an inner barrel so as to promote the primary crystallization of the allulose solution in the inner barrel;
s605, after the allulose 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 allulose solution in the inner barrel is cooled; and deeply crystallizing the primarily crystallized allulose solution in a vacuum environment until the crystallization is finished.
The invention has at least the following beneficial effects:
1. according to the invention, by arranging the inner barrel, the exchange cavity, the condenser and the like, when the psicose is purified, 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, so that heat is transferred to the inner barrel, and the psicose solution in the inner barrel enters an evaporation crystallization stage after being heated and heated; 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 to perform deep crystallization. In the process of evaporation crystallization, the heated evaporant of the psicose solution enters a condenser through a conveying pipe, is condensed and liquefied by the condenser and then enters a collection bin for uniform collection. The device is reasonable in structure, can heat or cool the inner barrel according to the allulose crystallization process to carry out evaporative crystallization and cooling deep crystallization, can control the vacuum degree in the inner barrel, promotes the crystallization of crystals in the supersaturated allulose solution, and improves the crystallization speed and quality of the allulose solution.
2. According to the invention, the crystal carrier is arranged and works together with the electromagnetic region, the stirring blades and the like, so that in the seed crystal adding process, after the seed crystal carrier falls off from the magnetic suction groove, the seed crystal carrier penetrates through the allulose solution and can fall onto the blades of the corresponding stirring blades, finally the magnetic attraction is carried out on the blades of the corresponding stirring blades, so as to ensure that the seed crystal in the seed crystal carrier can synchronously rotate with the corresponding blades, and in the process of rotating along with the blades, under the centrifugal force generated by the rotation of the blades and the impact resistance of the allulose solution, the allulose seed crystal in the seed crystal carrier can penetrate through the meshes of the porous net and is uniformly dispersed into the allulose solution.
3. According to the invention, the collection bin, the condenser, the weighing unit, the electromagnetic region, the crystal carrier and the stirring blade work cooperatively, on one hand, the weight of an evaporated substance in an evaporation crystallization stage is measured through the condenser and the weighing unit, and the weight is used as a condition for judging that the allulose solution reaches the metastable region of the supersaturated solution while the evaporated substance is recycled and is used as a condition for triggering the electromagnetic region to release the crystal carrier; after the crystal carrier is separated from the electromagnetic region, the crystal carrier is further magnetically adsorbed on the blades of the corresponding stirring blades, and in the rotating process of the blades of the stirring blades, under the centrifugal force generated by the rotation of the blades and the resistance impact effect of the allulose solution, the allulose seed crystals in the seed crystal carrier can penetrate through meshes of the porous net and are uniformly dispersed in the allulose solution, so that the multipoint and dynamic addition of the allulose seed crystals is realized, the distribution uniformity of the allulose seed crystals 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 needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the top cover and purification bin of the present invention;
FIG. 3 is a schematic view of the structure of a purification chamber and an exchange chamber according to the present invention;
FIG. 4 is a schematic view of a driving portion according to the present invention;
FIG. 5 is a schematic view of the structure of the magnetic field and the magnetic slot on the top cover of the present invention;
FIG. 6 is a schematic diagram of a crystal support structure according to the present invention;
FIG. 7 is a schematic view of the structure of the stirring blade and the rotating shaft of the present invention;
FIG. 8 is a schematic top view of the crystal carrier magnetically attached to the stirring blade of the present invention;
FIG. 9 shows a flow chart of the allulose purification process of the present invention.
In the figure: 1. a drive section; 101. butting a screw rod; 102. mounting a plate; 103. a motor; 104. a fixed block; 105. a rotating shaft; 106. fixing the screw rod; 107. butting nuts; 108. a butt joint block; 2. a crystal support; 201. an upper counterweight portion; 202. a lower weight portion; 203. a collar; 204. a porous web; 3. a carrier plate; 4. a purification bin; 5. a delivery pipe; 6. a condenser; 7. sleeving and clamping; 8. a support frame; 9. a collection bin; 10. a feed pipe; 11. a stirring blade; 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
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and 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.
Example 1
As shown in fig. 1-4, a purification device for producing psicose comprises a purification bin 4, an inner barrel 16 is detachably connected inside the purification bin 4, and the inner barrel 16 is used for crystallization and purification of psicose solution; 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, the hot water is introduced for heating when the psicose solution is evaporated and crystallized to evaporate, and then the cold water is introduced for cooling to perform deep crystallization. The top edge of the purification bin 4 is detachably connected with a cover plate 17 matched with the exchange cavity 14, and the two sides of the top of the cover plate 17 are symmetrically provided with 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; hot water or cold water can be introduced through the water inlet pipe 15 and the water outlet pipe 18 according to the crystallization process of the psicose to realize heat exchange so as to correspondingly carry out evaporation crystallization and cooling crystallization.
The top of purification storehouse 4 can be dismantled and be connected with top cap 13, and top cap 13's top one side intercommunication has inlet pipe 10, and the opposite side intercommunication has outlet duct 12. The feed pipe 10 is used to add the allulose solution into the inner barrel 16.
The inner chamber bottom center department of interior bucket 16 is provided with rabbling mechanism, and rabbling mechanism is including running through interior bucket 16 and purification storehouse 4 seal assembly and pivot 105, and pivot 105 is connected with drive division 1, can drive the rabbling mechanism through drive division 1 and pivot 105 and rotate to stir the allulose solution in the purification storehouse 4, guarantee that the allulose solution in the purification storehouse 4 is heated evenly, do benefit to the crystallization of allulose crystal, improve crystallization quality.
The bottom of one side of the purification bin 4 is connected with a collection bin 9 through a bottom plate, a vacuum pump is arranged in the collection bin 9, on one hand, the vacuum pump can vacuumize the upper part in the inner barrel 16 to promote the crystallization of crystals in the supersaturated allulose solution; on the other hand, in the evaporative crystallization stage, the evaporated material of the allulose solution can be sucked into the collection chamber 9.
The top of collecting the storehouse 9 is provided with condenser 6, and the output of condenser 6 is linked together with the inside of collecting the storehouse 9, and the input of condenser 6 passes through conveyer pipe 5 and outlet duct 12 intercommunication. In the process of evaporation and crystallization of the allulose solution in the purification bin 4, evaporated substances are pumped to the condenser 6 through the vacuum pump, the conveying pipe 5 and the air outlet pipe 12, are liquefied through the condensation effect of the condenser 6, and are finally collected into the collection bin 9 to be reused.
In the process of evaporating and crystallizing the psicose solution and cooling the solution in a vacuum environment to separate and obtain the psicose crystal, the temperature and the vacuum degree during crystallization are the most critical factors, and the psicose solution enters a high-over-saturation state due to overhigh or overlow temperature and overhigh vacuum degree, so that the granularity of crystal particles is reduced, and the yield and the purity of the crystal are influenced; and too high temperature can also cause psicose denaturation and also affect purity; therefore, in the process of allulose concentration, temperature reduction and separation for crystallization, two external conditions of temperature and vacuum degree need to be strictly controlled to ensure the crystallization purity of allulose; in the device, through the arrangement of the exchange cavity 14 and the inner barrel 16, when the allulose needs to be crystallized and purified, the allulose 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, so that heat is transferred to the inner barrel 16, and an allulose solution in the inner barrel 16 enters an evaporation crystallization stage after being heated and heated; according to the crystallization process of the psicose solution, circulating cold water is introduced into the exchange cavity 14 through the water inlet pipe 15 and the water outlet pipe 18, and the psicose solution in the inner barrel 16 is cooled for deep crystallization.
In the process of evaporation and crystallization, the heated evaporant of the psicose solution enters a condenser 6 through a conveying pipe 5, is condensed and liquefied by the condenser, and then enters a collection bin 9 for uniform collection. This device is rational in infrastructure, can heat or cool down interior bucket 16 according to psicose crystallization process to evaporating crystallization and cooling degree of depth crystallization, and can control the vacuum in interior bucket 16, promoting the crystal crystallization in the psicose solution of supersaturation, improve the speed and the quality of psicose solution crystallization.
Further, the bottom of interior bucket 16 and the inner chamber bottom bolt fixed connection of purification storehouse 4, top cap 13 and the top looks sealing connection of purification storehouse 4, it is concrete, through the setting of interior bucket 16, be convenient for clear up inside impurity comprehensively.
Further, the jacket clamp 7 is sleeved on the outer ring of the condenser 6, the supporting frames 8 fixedly connected with the bottom plate bolts and fixedly connected with the two sides of the jacket clamp 7 are fixedly connected, and particularly, the installation stability of the condenser 6 is guaranteed through the arrangement of the supporting frames 8.
Further, 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 and installs the motor 103 in the loading board 3 bottom through mounting panel 102, and the output shaft of motor 103 is connected with the tip transmission of pivot 105, and is concrete, 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 clamping screw 106 that one end runs through mounting panel 102, clamping screw 106's one end bolt fixedly connected with and 3 bottom fixed connection's of loading board fixed block 104, other end fixedly connected with butt joint piece 108, the bottom level of mounting panel 102 is provided with butt joint screw 101, the one end of butt joint screw 101 runs through two butt joint piece 108 threaded connection and has butt joint nut 107, specifically, through the setting of mounting panel 102, be convenient for carry out the dismouting to motor 103, the later stage dimension of being convenient for is protected and is transported.
In summary, the following steps: when allulose needs to be purified, allulose is added into an inner barrel 16 through a feed pipe 10, a water inlet pipe 15 and a water outlet pipe 18 are opened to introduce circulating hot water into an exchange cavity 14, so that heat is transferred to the inner barrel 16, allulose solution in the inner barrel 16 is heated and 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 14 through the water inlet pipe 15 and the water outlet pipe 18, and the psicose solution in the inner barrel 16 is cooled for deep crystallization. In the process of evaporation and crystallization, the heated evaporant of the psicose solution enters a condenser 6 through a conveying pipe 5, is condensed and liquefied by the condenser, and then enters a collection bin 9 for uniform collection. This device is rational in infrastructure, can heat or cool down interior bucket 16 according to psicose crystallization process to evaporating crystallization and cooling degree of depth crystallization, and can control the vacuum in interior bucket 16, promoting the crystal crystallization in the psicose solution of supersaturation, improve the speed and the quality of psicose solution crystallization.
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 allulose solution. For the allulose solution with high solution viscosity, crystal nuclei are difficult to generate, and when crystallization is carried out under high supersaturation degree, the crystal nuclei are fast in forming rate, so that the polycrystalline phenomenon is easy to occur, and the product quality is not easy to control. Therefore, a high-viscosity solution of psicose must be prepared by seeding the metastable region. Therefore, the seeding must be done at a good time, with the solution entering the metastable zone at the appropriate temperature, and with gentle agitation to spread the seeds evenly throughout the solution. The device is therefore further developed for achieving the above-mentioned objects.
As shown in fig. 5-8, an electromagnetic area 19 is disposed 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 the 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, the lower counterweight part 202 is connected with a lantern ring 203, and the lantern ring 203 is connected with the upper counterweight part 201 through a porous net 204; before seed crystal is added, the allulose seed crystal can be poured into the lantern ring 203 through the porous net 204, then the electromagnetic region 19 is controlled by the control system to be electrified to generate magnetism, the magnetic absorption groove 20 is magnetized, then the crystal carrier 2 is magnetically absorbed in the magnetic absorption groove 20 through the upper counterweight part 201, and preparation is made in advance for adding the allulose seed crystal. The upper counterweight 201 and the lower counterweight 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 blades when entering the psicose solution of the inner barrel 16.
Specifically, the pore size of the porous mesh 204 is larger than the particle size of the psicose crystals, so as to ensure that the psicose crystals can penetrate through the meshes of the porous mesh 204 and be uniformly dispersed into the psicose solution when the seeds are added subsequently.
Specifically, be equipped with the stirring vane 11 of multiunit magnetism material on the pivot 105, and the blade of two sets of adjacent stirring vane 11 is the setting of interlocking each other, stirring vane 11's blade quantity equals with crystal carrier 2's quantity, when stirring vane 11 is located the initial position, stirring vane 11's blade and crystal carrier 2 one-to-one, so that at the in-process that adds the seed crystal, after seed crystal carrier 2 drops from magnetism groove 20, seed crystal carrier 2 passes allulose solution and can fall on corresponding stirring vane 11's blade, final magnetism adsorbs on corresponding stirring vane 11's blade, in order to guarantee that follow-up corresponding blade synchronous rotation.
Further, the motor 103 adopts servo motor to guarantee that the initial position can both be reached when the accurate control motor 103 stops at every turn, and the blade on the stirring vane 11 can be corresponding with the crystal carrier 2 that corresponds mutually one-to-one when the initial position, in order to guarantee that the crystal carrier 2 can be adsorbed on the blade of corresponding stirring vane 11 by the magnetism after coming off from the electromagnetic zone 19.
Specifically, stirring vane 11 is equipped with two sets ofly, the blade quantity on every group stirring vane 11 is four, and stirring vane 11's blade total number equals crystal carrier 2's total number, guarantee like this that crystal carrier 2 is after the magnetism adsorbs to the blade, can follow the blade and rotate the in-process, under centrifugal force and the allulose solution resistance impact effect that the blade rotation produced, the allulose seed crystal in the seed crystal carrier 2 can pass the mesh of many empty nets 204, even dispersion has realized the multiple spot of allulose seed crystal, the developments are added, further improve the homogeneity of distribution of allulose seed crystal in the solution greatly, improve the effect of follow-up crystallization.
A weighing unit is arranged below the collection bin 9; the weighing unit is used for weighing the increased weight of the collecting bin 9; by setting a preset value of the weighing unit in the control system, the allulose solution in the inner barrel 16 reaches a metastable zone of supersaturated solution when the weighing unit measures that the weight of the collecting bin 9 reaches the preset value. Since the allulose 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 a metastable zone. The evaporated substances are filled into the condenser 6 through the vacuum pump, the conveying pipe 5 and the air outlet pipe 12 to be condensed and liquefied, and then are collected into the collecting bin 9; the weight of the evaporation material collected into the collection bin 9 is calculated through the weighing unit, whether the psicose solution forms a saturated solution or not can be judged and the solution enters a metastable zone (the solution with a certain concentration can be understood, the amount of the solvent evaporated when the saturated concentration is reached through heating evaporation can be calculated and measured), the weighing unit is used for calculating the weight increment of the collection bin 9 to set a preset value, the time for adding the psicose seed crystal is guaranteed, namely, when the weighing unit detects that the weight of the collection bin 9 reaches the preset value, the psicose solution in the purification bin 4 reaches the metastable zone of the supersaturated solution, the seed crystal is added at the moment, the crystallization rate can be improved, and the quality of the crystallized product is guaranteed.
Through the improvement of 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 the allulose in the inner barrel 16, the vacuum pump and the conveying pipe 5 vacuumize the inner barrel 16, and evaporated substances are condensed by the condenser 6 and then are recovered into the collecting bin 9; when the weighing unit detects that the weight of the collecting bin 9 reaches a preset value, the control system controls the electromagnet in the electromagnetic region 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 penetrates through the psicose solution and then is magnetically adsorbed on the stirring blade 11, and the stirring blade 11 drives the crystal carrier 2 to rotate, so that the psicose crystals in the crystal carrier 2 penetrate through the porous net 204 and are uniformly dispersed into the inner barrel 16.
In conclusion, the collecting bin 9, the condenser 6 and the weighing unit cooperate with the electromagnetic region 19, the crystal carrier 2 and the stirring blade 11 to work cooperatively, so that on one hand, the weight of an evaporated substance in an evaporation crystallization stage is measured by the condenser and the weighing unit, the evaporated substance is recycled and reused, and meanwhile, the condition for judging that the allulose solution reaches a metastable region of a supersaturated solution is used as the condition for triggering the electromagnetic region 19 to release the crystal carrier 2; after the crystal carrier 2 is separated from the electromagnetic region, the crystal carrier is further magnetically adsorbed on the corresponding blade of the stirring blade 11, and in the rotating process of the blade of the stirring blade 11, under the centrifugal force generated by the rotation of the blade and the resistance impact effect of the allulose solution, the allulose seed crystals in the seed crystal carrier 2 can pass through the meshes of the porous net 204 and be uniformly dispersed in the allulose solution, so that the multipoint and dynamic addition of the allulose seed crystals is realized, the distribution uniformity of the allulose seed crystals in the solution is further greatly improved, and the subsequent crystallization effect is improved.
Example 3
The invention also provides a method for purifying psicose, which adopts a purification device to purify the psicose, as shown in fig. 9, and comprises the following steps:
s1, adopting crystalline glucose as a raw material, and converting the crystalline glucose by isomerase to obtain high fructose syrup;
s2, after the high fructose corn syrup is decolorized and ion-exchanged, separating the high fructose corn syrup by a high-efficiency simulated moving bed to obtain high fructose syrup with fructose content more than 98 percent;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain a fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup by using epimerase;
s5, separating the fructose and psicose mixed syrup by 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 crystallized allulose from the mother liquor, drying and screening allulose crystals to obtain allulose crystal products; the separated mother liquor is recycled.
Wherein, the step of S6 specifically comprises the following steps:
s601, injecting the psicose solution into the inner barrel 16 through the feed pipe 10, opening the water inlet pipe 15 and the water outlet pipe 18 to introduce circulating hot water into the exchange cavity 14, heating the psicose solution in the inner barrel 16, and carrying out evaporation crystallization;
s602, starting a vacuum pump, vacuumizing the interior of the inner barrel 16, pumping evaporated substances to a condenser 6 through a conveying pipe 5 and an air outlet pipe 12, condensing and liquefying the evaporated substances through the condenser 6, and collecting the condensed substances into a collecting bin 9;
s603, when the weighing unit detects 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 in the electromagnetic area 19 falls off and descends into the inner barrel 16;
s604, magnetically adsorbing the crystal carrier 2 separated from the electromagnetic region 19 on the stirring blade 11, and driving the crystal carrier 2 to rotate by the stirring blade 11, so that the allulose crystals in the crystal carrier 2 pass through the porous net 204 and are uniformly dispersed into the inner barrel 16, and primary crystallization of the allulose solution in the inner barrel 16 is promoted;
s605, after the allulose 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 allulose solution in the inner barrel 16 is cooled, and the primarily crystallized allulose solution is deeply crystallized in a vacuum environment until the crystallization is completed.
The foregoing shows and describes the general principles, essential 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, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A purification device for producing psicose comprises a purification bin and is characterized in that an inner barrel is detachably connected inside the purification bin, an exchange cavity is arranged between the purification bin and the inner barrel, a cover plate matched with the exchange cavity is detachably connected at the edge of the top of the purification bin, and water inlet pipes and water outlet pipes which penetrate through the cover plate and are communicated with the inside of the exchange cavity are symmetrically arranged on 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 feeding 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 absorption grooves are uniformly arranged in a matrix manner in the electromagnetic area, and crystal carriers are magnetically absorbed in the magnetic absorption grooves;
the crystal carrier comprises an upper counterweight part and a lower counterweight part which are made of ferromagnetic materials, 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;
a stirring mechanism is arranged at the center of the bottom of the inner cavity of the inner barrel and comprises a sealing assembly and a rotating shaft, the sealing assembly penetrates through the inner barrel and the purification bin, a plurality of groups of magnetic stirring blades are arranged on the rotating shaft, blades of two adjacent groups of stirring blades are arranged in a staggered mode, the number of the blades 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 interior 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 allulose in the inner barrel, simultaneously, the inner barrel is vacuumized through the vacuum pump and the conveying pipe, and evaporated substances are condensed by the condenser and then are recovered into the collection bin; when the weighing unit records 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, the crystal carrier magnetically adsorbed by the magnetic attraction groove falls off and descends into the inner barrel, then the crystal carrier is magnetically adsorbed on the stirring blade, and the stirring blade drives the crystal carrier to rotate, so that the psicose crystals in the crystal carrier penetrate through the porous net and are uniformly dispersed into the inner barrel.
2. A purification apparatus for psicose production according to claim 1, wherein the psicose solution in the inner barrel reaches a metastable zone of supersaturated solution when the weight of the collection bin measured by the weighing unit reaches a preset value.
3. A purification apparatus for psicose production 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.
4. A purification apparatus for producing psicose according to claim 1, wherein the porous mesh has a pore size larger than the particle size of the psicose crystals.
5. The purification device for producing psicose of claim 1, wherein the bottom of the inner barrel is fixedly connected with the bottom of the inner cavity of the purification bin by bolts, and the top cover is hermetically connected with the top of the purification bin.
6. The purification device for producing allulose of claim 1, wherein a jacket clamp is sleeved on an outer ring of the condenser, and supporting frames fixedly connected with bottom plate bolts are fixedly connected to two sides of the jacket clamp.
7. The purification device for producing allulose according to claim 1, wherein a bearing plate is arranged below the purification bin, a driving part is arranged at the bottom of the bearing plate, the driving part comprises a motor mounted at the bottom of the bearing plate through a mounting plate, and an output shaft of the motor is in transmission connection with an end of the rotating shaft.
8. The purification device for producing allulose according to claim 7, wherein the mounting plate is provided with a fixing screw at both sides of the bottom thereof, one end of the fixing screw penetrates through the mounting plate, one end of the fixing screw is fixedly connected with a fixing block fixedly connected with the bottom of the bearing plate through a bolt, the other end of the fixing screw is fixedly connected with a butt block, the bottom of the mounting plate is horizontally provided with a butt screw, and one end of the butt screw penetrates through two butt blocks and is connected with a butt nut through threads.
9. A purification method of psicose, which purifies psicose using the purification apparatus according to any one of claims 1 to 8, comprising the steps of:
s1, adopting crystalline glucose as a raw material, and converting the crystalline glucose by isomerase to obtain high fructose syrup;
s2, after the high fructose corn syrup is decolorized and ion-exchanged, separating the high fructose corn syrup by a high-efficiency simulated moving bed to obtain high fructose syrup with fructose content more than 98 percent;
s3, concentrating, crystallizing and separating the high fructose syrup to obtain crystalline fructose, and performing secondary crystallization to obtain a fructose crystallization mother liquor;
s4, converting the fructose crystallization mother liquor into fructose and psicose mixed syrup by using epimerase;
s5, separating the fructose and psicose mixed syrup by 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 crystallized allulose from the mother liquor, drying and screening allulose crystals to obtain allulose crystal products; the separated mother liquor is recycled.
10. The method for purifying psicose according to claim 9, wherein the step S6 comprises the following steps:
s601, injecting the psicose solution into an inner barrel through a feed pipe, opening a water inlet pipe and a water outlet pipe to introduce circulating hot water into an exchange cavity, heating the psicose solution in the inner barrel, and carrying out evaporative crystallization;
s602, starting a vacuum pump, vacuumizing the inner barrel, pumping evaporated substances to a condenser through a conveying pipe and an air outlet pipe, condensing and liquefying the evaporated substances through the condenser, and collecting the condensed substances into a collection 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, adsorbing the crystal carrier magnetic separated from the electromagnetic region on a stirring blade, and driving the crystal carrier to rotate by the stirring blade to enable the allulose crystals in the crystal carrier to penetrate through a porous net and be uniformly dispersed into an inner barrel so as to promote the primary crystallization of the allulose solution in the inner barrel;
s605, after the allulose 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 allulose solution in the inner barrel is cooled; and deeply crystallizing the primarily crystallized allulose solution in a vacuum environment until the crystallization is finished.
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CA3042033A1 (en) * 2016-10-28 2018-05-03 Tate & Lyle Ingredients Americas Llc Method for producing allulose crystals
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CN110627847A (en) * 2019-09-17 2019-12-31 山东百龙创园生物科技股份有限公司 Preparation method of psicose crystal
CA3121460A1 (en) * 2018-11-30 2020-06-04 Cj Cheiljedang Corporation D-psicose crystal and preparation method therefor
CN112321654A (en) * 2020-11-05 2021-02-05 江西诚志生物工程有限公司 Raw material purification and impurity removal method for D-ribose production

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07251003A (en) * 1994-03-14 1995-10-03 Nisshin Flour Milling Co Ltd Crystalization method by reaction using gel
KR20160046143A (en) * 2014-10-20 2016-04-28 씨제이제일제당 (주) A method of manufacturing a d-psicose crystal
US20190177351A1 (en) * 2014-10-20 2019-06-13 Cj Cheiljedang Corporation Method for preparing d-psicose crystal
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