CN108176074B - Progressive freeze concentration equipment with double-sandwich structure and freeze concentration method - Google Patents
Progressive freeze concentration equipment with double-sandwich structure and freeze concentration method Download PDFInfo
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- CN108176074B CN108176074B CN201810188990.4A CN201810188990A CN108176074B CN 108176074 B CN108176074 B CN 108176074B CN 201810188990 A CN201810188990 A CN 201810188990A CN 108176074 B CN108176074 B CN 108176074B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention relates to progressive freeze concentration equipment with a double-sandwich structure, which comprises a crystallization concentration unit, a cold carrier temperature control unit and a parameter control and automatic recording unit, wherein the crystallization concentration unit is connected with the cold carrier temperature control unit; the crystallization concentration unit comprises a crystallization concentration tank, an outer interlayer temperature probe and a plurality of groups of temperature recording probes in the tank; the side wall of the crystallization concentration tank is of a double-sandwich structure and comprises an inner sandwich layer communicated with a buffer heat transfer carrier I and an outer sandwich layer communicated with a cold carrier II, wherein the carrier I is a food-grade carrier with heat transfer buffer characteristics, and the cold carrier II is an anti-freezing cold carrier; the outer interlayer temperature probe is arranged in the outer interlayer; the temperature recording probes are arranged in the crystallization concentration tank. The invention also relates to a freeze concentration method. The equipment can realize stable and accurate control of the temperature of the feed liquid in the freeze concentration process, and has the advantages of good freeze concentration effect, strong universality for different feed liquids, high automation degree, contribution to optimizing process conditions and the like.
Description
Technical Field
The invention belongs to the technical field of low-temperature processing, and particularly relates to progressive freezing and concentrating equipment with a double-sandwich structure and a concentrating method.
Background
Freeze concentration is a liquid material concentration technique commonly used in the industries of food, nutraceuticals, biopharmaceuticals and the like and operated below freezing point. Compared with the evaporation concentration technology, the method has great advantages in the aspects of effectively recycling the heat-sensitive natural aromatic flavor substances, proteins, enzymes, polysaccharide, polyphenol, water-soluble vitamins and other bioactive components of the liquid materials. Freeze concentration can be divided into two major technical systems, suspension and progressive, depending on the different ways of ice core formation and ice crystal removal in solution. The suspension type freezing and concentrating equipment has very complex structure and high manufacturing cost, and is limited in production and application investment. The progressive freeze concentration is different from the traditional suspension freeze concentration in operation principle, and the solution in the crystallization tank forms a large ice crystal layer on the other side of the cold carrier layer, and the solution is concentrated along with the gradual thickening of the ice layer. The progressive freezing and concentrating process has the obvious characteristic that ice crystals form one flaky or annular ice crystal in the crystallizing tank, the solid-liquid interface is small, the separation of the ice crystals and the concentrated solution is easy, the solute loss caused by the entrainment of the ice crystals can be reduced, the generation and growth of the ice crystals and the separation of the ice crystals and the concentrated solution are completed in one system, the equipment structure is relatively simple, and the operation is convenient. At present, progressive freeze concentration at home and abroad has evolved into a tube type, falling film type, partial icing type, rotary drum type, belt type and other concentration devices based on different operation modes.
Existing progressive freeze concentration related devices or methods are mostly based on cold carrier single-layer wrapped crystallization concentration tank structures, and mostly lack cold carrier temperature control devices and operating parameter control and recording systems, such as: the preparation method of the clear concentrated juice disclosed in CN 104886702A uses a cold carrier single interlayer stirring type progressive local freezing and concentrating tank, and the freezing, concentrating and crystallizing tank can realize freezing of feed liquid in the tank, but is difficult to overcome generation of dendritic heterogeneous ice crystals and can influence the concentrating effect because a cold carrier interlayer temperature control device is not arranged. In addition, other progressive freeze concentration techniques are presently disclosed, such as: the advanced freeze concentration control method disclosed in CN 1593248A uses a single-interlayer pipe type circulating progressive freeze concentration device; the 'small freezing and concentrating equipment' disclosed in CN 1442222A belongs to a progressive freezing and concentrating device with partially frozen bottom; the "freezing and concentrating process of vinegar" disclosed in CN 104178408A and the "freezing and concentrating method of fruit juice" disclosed in CN 101991157A are both simple methods of freezing fruit juice or vinegar in a refrigerator or a refrigerator and then thawing, and lack of accurate control of operation parameters of the freezing and concentrating processes.
It follows that existing progressive freeze concentration devices or apparatus suffer from the following problems:
1) The lack of accurate and stable control of the temperature change rate of the cold carrier of the crystallization tank influences the freezing concentration effect. In order to realize continuous cooling of the feed liquid, the interlayer of the cold carrier of the crystallization tank is required to continuously provide cooling capacity for the feed liquid in the tank, if accurate and stable control of the temperature of the cold carrier is not available, the feed liquid in the tank, which is close to the wall surface, is often caused to have larger local supercooling degree, dendritic heterogeneous ice crystals are formed, higher branches (namely secondary nucleation) are generated on trunk branches, solute molecules are wrapped, the entrainment capacity of the solute is increased, and the concentration effect is seriously affected.
2) The lack of precise and stable control of the rate of change of the temperature of the frozen concentrate feed solution results in a device that has low versatility for frozen concentrate of liquids of different types of morphology.
3) The lack of scientific treatment means in the late thawing stage affects the production efficiency. After progressive freeze concentration is finished, the ice-entrained defrosting process is carried out, natural defrosting of large ice cubes in the heat preservation system is very slow, even days are required, and the production efficiency of equipment is seriously affected.
4) The lack of a real-time recording function of the whole-process operation process parameters is unfavorable for analysis and optimization of the freeze concentration process conditions.
Disclosure of Invention
Based on the above, the invention aims to provide the progressive freeze concentration equipment with the double-sandwich structure, which can realize stable and accurate control of the temperature of feed liquid in the freeze concentration process and has the advantages of good freeze concentration effect, strong universality for different feed liquids, high automation degree, contribution to optimizing process conditions and the like.
The technical scheme adopted by the invention is as follows:
a progressive freeze concentration device with a double-sandwich structure comprises a crystallization concentration unit, a cold carrier temperature control unit and a parameter control and automatic recording unit;
the crystallization concentration unit comprises a crystallization concentration tank, an outer interlayer temperature probe and a plurality of groups of temperature recording probes; the side wall of the crystallization concentration tank is of a double-sandwich structure and comprises an inner sandwich layer communicated with a carrier I and an outer sandwich layer communicated with a cold carrier II, wherein the carrier I is a food-grade carrier with heat transfer buffering characteristics (the food-grade carrier with the heat conductivity coefficient of 0.02-0.20 w/m DEG C), and the cold carrier II is an anti-freezing cold carrier (a mixed solution consisting of propylene glycol, ethanol and water); the outer interlayer temperature probe is arranged in the outer interlayer; the temperature recording probes are arranged in the crystallization concentration tank;
the cold carrier temperature control unit comprises a cold carrier tank filled with a cold carrier II, a temperature balance control box, a refrigeration compressor, a heat exchanger, a first low-temperature circulating pump and a second low-temperature circulating pump; the cold carrier tank, the temperature balance control box and the outer interlayer are connected through a pipeline to form a circulation loop (called 'outer circulation') for circulating the cold carrier II, and the first low-temperature circulation pump is arranged on the pipeline between the cold carrier tank and the temperature balance control box; the cold carrier tank and a heat medium channel in the heat exchanger are connected through a pipeline to form a circulation loop (called 'cooling internal circulation') for circulating a cold carrier II, the second low-temperature circulation pump is arranged on a pipeline between the cold carrier tank and the heat exchanger, and low-temperature refrigerant generated by the refrigeration compressor is introduced into the refrigerant channel in the heat exchanger;
the parameter control and automatic recording unit comprises an operation parameter panel, a controller and an operation data recording storage, wherein the operation parameter panel and the operation data recording storage are respectively and electrically connected with the controller; the controller is electrically connected with the outer interlayer temperature probe, the plurality of groups of temperature recording probes, the first low-temperature circulating pump, the second low-temperature circulating pump and the refrigeration compressor respectively.
Compared with the prior art, the progressive freeze concentration device has the following beneficial effects:
1) The stable control of the temperature of the feed liquid and the change rate thereof is realized in the freezing and concentrating process.
The crystallization concentration tank with the double-interlayer structure is adopted, and in the freezing concentration stage, the temperature of feed liquid in the tank can be steadily reduced through the conduction fit between the carrier I with heat transfer buffer characteristics in the inner interlayer and the anti-freezing cold carrier II in the outer interlayer. Meanwhile, through double control of external circulation and cooling internal circulation of the cold carrier II, the temperature change of the cold carrier II input into the external interlayer is effectively ensured to be very stable, so that the stable reduction of the temperature of the feed liquid to be concentrated in the tank is realized, pure ice crystals are favorably formed, dendritic heterogeneous ice crystals are prevented from being formed due to overlarge rate of the reduction of the temperature of the feed liquid in the tank, and the ideal concentration effect is achieved.
2) The accurate control of the temperature of the feed liquid and the change rate thereof is realized in the freezing and concentrating process.
The temperature ranges of each cooling stage can be preset by utilizing the operation parameter panel in the parameter control and automatic recording unit, and the running states of the external circulation and the cooling internal circulation in the cold carrier temperature control unit are controlled by the controller, so that the feed liquid in the tank can reach the set temperature in each cooling stage, the accurate control of the feed liquid temperature dropping rate is realized, and the concentration effect is improved. The equipment can realize that the temperature difference between the axial center of the feed liquid in the tank and each position between the inner wall of the tank reaches 0.0-15.0 ℃.
3) The degree of automation is high.
The parameter control and automatic recording unit is adopted, the temperature range of the cold carrier tank, the temperature range of the temperature balance control box, the conveying speed of the first low-temperature circulating pump, the conveying speed of the second low-temperature circulating pump, the power of the refrigeration compressor and other technological parameters can be set in stages through the operation parameter panel according to the freezing concentration process, and the controller provided with parameter management software is utilized to automatically operate and control all electric components in the operation process.
4) The universality for different feed liquids is strong.
The requirements of the freeze concentration process of feed liquid with different varieties, different concentrations and different components are obviously different. The equipment can stably and accurately control the temperature and the change rate of the feed liquid, so that the equipment can meet the freezing and concentrating process requirements of feed liquids with different properties, and realize the effective concentration of the feed liquids with different properties.
5) Is beneficial to optimizing the process conditions.
Real-time data of operation process parameters of each character feed liquid in the freeze concentration process is important data for analyzing and re-optimizing the freeze concentration process conditions, so that the recording and storage functions of the operation data of the equipment are very important. By setting the operation data record storage, the real-time change value of the process parameter in the whole freezing concentration process can be recorded according to the set recording time frequency, and the operation data can be exported and edited by connecting a router or a transmission line with a computer, so that the process condition can be conveniently analyzed and optimized.
Further, the crystallization concentration unit further comprises a pneumatic lifting device, the pneumatic lifting device comprises two lifting rods, a belt Kong Binghuan supporting plate and an air cylinder, the two lifting rods extend into the crystallization concentration tank, the bottom ends of the two lifting rods are fixedly connected with the belt Kong Binghuan supporting plate respectively, and the top ends of the two lifting rods are connected with the power output end of the air cylinder.
Through this pneumatic lifting device, can go up and down the ice ring that the periphery has slightly thawed in the stage of thawing, conveniently in time unload the ice ring outward, realize the external quick thawing of jar, solve the interior big ice-cube of insulation system and naturally defrost very slow problem, save a large amount of time, improve production efficiency.
Further, the crystallization concentration unit also comprises a heat preservation material cylinder and a low-temperature pump; the bottom of the crystallization concentration tank is provided with a feed liquid inlet valve communicated with the tank, the top of the inner interlayer is provided with a carrier I inlet valve communicated with the inside of the inner interlayer, and the bottom of the inner interlayer is provided with a carrier I outlet valve communicated with the inside of the inner interlayer; the bottom of the heat-preservation material cylinder is provided with a material liquid outlet, and the material liquid outlet is respectively connected with the feeding end of the low-temperature pump and the carrier I inlet valve through pipelines; the feeding end of the cryogenic pump is connected with the carrier I outlet valve through a pipeline, the discharging end of the cryogenic pump is connected with the feed liquid inlet valve through a pipeline and is connected with a circulating pipeline extending into the heat-preserving material cylinder, and a circulating control valve is arranged on the circulating pipeline.
Through setting up heat preservation feed cylinder, cryopump, circulation pipeline and above-mentioned pipeline connected mode, on the one hand be convenient for wash the crystallization concentration jar, advance the operation of waiting concentrated feed liquid, on the other hand, after thawing stage discharge concentrated mother liquor, usable cryopump changes the medium in the inlayer into next batch and waits to concentrate feed liquid to make next batch wait to concentrate feed liquid circulation flow in the inlayer, thereby retrieve the cold volume that releases when ice ring thawing in the crystallization concentration jar, play the precooling of waiting to concentrate feed liquid and reduce the effect of energy consumption.
Further, the bottom of the outer interlayer is provided with a cold carrier II inlet pipe communicated with the inside of the outer interlayer, the top of the outer interlayer is provided with a cold carrier II outlet valve communicated with the inside of the outer interlayer, and the cold carrier II inlet pipe is provided with a temperature control electromagnetic valve electrically connected with the controller; and the cold carrier II inlet pipe is connected with the temperature balance control box, and the cold carrier II outlet valve is connected with the cold carrier tank through a pipeline.
By arranging the temperature control electromagnetic valve, the opening and closing states of the inlet pipe of the cold carrier II are controlled according to the temperature measured by the temperature probe of the outer interlayer, so that whether the cold carrier II is input into the outer interlayer or not is controlled.
Further, the plurality of groups of temperature recording probes are distributed between the axial center in the crystallization concentration tank and the inner wall at intervals, the horizontal distance between every two adjacent groups of temperature recording probes is 1-5 cm, and the distance between the outermost group of temperature recording probes and the inner wall of the crystallization concentration tank is 1-2 mm.
The temperature gradient change between the axial center position of the concentrated feed liquid in the tank and the position close to the inner wall of the tank can be recorded by the plurality of groups of temperature recording probes, and the temperature gradient change has important significance for researching the relation between the heat transfer rate of feed liquid with different properties, ice crystal morphology and solute entrainment quantity, optimizing the freezing concentration process conditions and the like.
Further, the crystallization concentration unit also comprises a stirring device, wherein the stirring device comprises a stirring paddle, a sealing device and a stirring motor, the stirring paddle is arranged in the crystallization concentration tank, and the top end of the stirring paddle is arranged on the top of the crystallization concentration tank through the sealing device and is connected with the power output end of the stirring motor; the controller is electrically connected with the stirring motor.
Another object of the present invention is to provide a freeze concentration method comprising the steps of:
(1) Measuring the freezing point and supercooling point of the feed liquid to be concentrated;
(2) Delivering the feed liquid to be concentrated into a crystallization concentration tank; the side wall of the crystallization concentration tank is of a double-interlayer structure with an inner interlayer and an outer interlayer, and stirring paddles are arranged in the tank;
(3) Filling the carrier I into the inner interlayer of the crystallization concentration tank; the carrier I is a food-grade carrier with heat transfer buffering characteristics;
(4) Inputting the cold carrier II into the outer interlayer of the crystallization concentration tank, keeping circulating flow, and simultaneously cooling the cold carrier II input into the outer interlayer by utilizing a refrigeration compressor and a heat exchanger; the cold carrier II is an anti-freezing cold carrier;
(5) The temperature of the feed liquid to be concentrated in the crystallization concentration tank is reduced in four stages by controlling the flow rate of the cold carrier II input into the outer interlayer, the working state of the refrigeration compressor and the rotating speed of the stirring paddle, and freezing concentration is carried out, so that an ice ring is formed in the tank; the first stage is to lower the temperature of the feed liquid to 1 ℃ above and below the freezing point value, the second stage is to lower the temperature of the feed liquid to 1 ℃ above and below the supercooling point value, the third stage is to lower the temperature of the feed liquid by 4-6 ℃ on the basis of the second stage, and the fourth stage is to continuously lower the temperature of the feed liquid on the basis of the third stage;
(6) When the feed liquid in the crystallization concentration tank reaches the target concentration, all the concentrated mother liquid in the tank is discharged and collected.
Further, the method also comprises the step (7): and stopping the working of the refrigeration compressor, discharging and collecting the higher concentration feed liquid which is thawed and oozed by the ice ring in the crystallization concentration tank, and stopping collecting when the average concentration of the collected mixed feed liquid does not meet the concentration requirement. The higher concentration feed liquid which is thawed and extravasated by the ice ring preferentially is collected, so that the waste can be reduced, and the yield of the concentrated liquid can be improved.
Further, the method also comprises the step (8): and (3) draining the carrier I in the inner interlayer of the crystallization concentration tank, cleaning the inner interlayer by using clear water, then inputting the next batch of feed liquid to be concentrated into the inner interlayer, keeping circulating flow, thawing the outer wall of an ice ring in the crystallization concentration tank, and pre-cooling the next batch of feed liquid to be concentrated.
The medium in the inner interlayer is converted into the next batch of feed liquid to be concentrated, which is favorable for recovering cold and reducing energy consumption.
Further, step (8) further comprises: after the next batch of concentrated feed liquid is precooled, an air-operated lifting device is used for supporting an ice ring in the crystallization concentration tank, the top of the tank is opened, and the ice ring is taken out; the pneumatic lifting device comprises two lifting rods, a belt Kong Binghuan supporting plate and an air cylinder, wherein the two lifting rods extend into the crystallization concentration tank, the bottom ends of the two lifting rods are fixedly connected with the belt Kong Binghuan supporting plate respectively, and the top ends of the two lifting rods are connected with the power output end of the air cylinder.
For a better understanding and implementation, the present invention is described in detail below with reference to the drawings.
Drawings
FIG. 1 is a schematic diagram of a crystallization concentration unit;
FIG. 2 is a schematic diagram of the connection of a cold carrier temperature control unit;
FIG. 3 is a schematic diagram of the connection control of the parameter control and automatic recording unit;
FIG. 4 is a graph showing the temperature change of fruit vinegar at different locations in the crystallization and concentration tank during freeze concentration and thawing in example 3;
FIG. 5 is a graph showing the temperature change of citrus juice at various locations in a crystallization and concentration tank during freeze concentration and thawing in example 4.
Detailed Description
Example 1: progressive freezing concentration equipment with double-sandwich structure
Referring to fig. 1 to 3, fig. 1 is a schematic structural diagram of a crystallization concentration unit, fig. 2 is a schematic connection diagram of a cold carrier temperature control unit, and fig. 3 is a schematic connection control diagram of a parameter control and automatic recording unit.
The progressive freeze concentration device with the double-sandwich structure comprises a crystallization concentration unit, a cold carrier temperature control unit and a parameter control and automatic recording unit.
As shown in fig. 1, the crystallization concentration unit comprises a crystallization concentration tank 10, a heat preservation material cylinder 11, a cryopump 12, a pneumatic lifting device 13, a stirring device 14, an outer interlayer temperature probe 15 and a plurality of groups of temperature recording probes 16.
The top of the crystallization concentration tank 10 can be opened and closed, the tank bottom is provided with a feed liquid inlet valve 101 and a concentrated liquid discharge valve 102 which are communicated with the tank, and the top of the side wall is provided with an exhaust valve 103 which is communicated with the tank. The side wall of the crystallization concentration tank 10 is of a double-sandwich structure, and comprises an inner sandwich layer 104 communicated with a carrier I and an outer sandwich layer 105 communicated with a cold carrier II. The carrier I is a food-grade carrier with heat transfer buffering characteristics, and the cold carrier II is an anti-freezing cold carrier.
The top of the inner interlayer 104 is provided with a carrier I inlet valve 104a communicated with the inside of the inner interlayer, and the bottom of the inner interlayer is provided with a carrier I outlet valve 104b communicated with the inside of the inner interlayer. The bottom of the outer interlayer 105 is provided with a cold carrier II inlet pipe communicated with the inside of the outer interlayer 105, the cold carrier II inlet pipe is provided with a temperature control electromagnetic valve 105a, the top of the outer interlayer 105 is provided with a cold carrier II outlet valve 105b communicated with the inside of the outer interlayer 105,
the bottom of the heat preservation material cylinder 11 is provided with a material liquid outlet, and the material liquid outlet is respectively connected with the feeding end of the cryopump 12 and the carrier I inlet valve 104a through pipelines.
The feeding end of the cryopump 12 is connected with the outlet valve 104b of the carrier I through a pipeline, the discharging end of the cryopump 12 is connected with the feed liquid inlet valve 101 through a pipeline and is connected with a circulating pipeline 17 extending into the heat insulation material cylinder 11, and a circulating control valve 170 is arranged on the circulating pipeline 17.
The pneumatic lifting device 13 comprises two lifting rods 131, a supporting plate 132 with a Kong Binghuan belt and an air cylinder. The two lifting rods 131 extend into the crystallization concentration tank 10, the bottom ends of the two lifting rods are fixedly connected with the supporting plates 132 of the belts Kong Binghuan respectively, and the top ends of the two lifting rods are connected with the power output end of the air cylinder. The cylinder controls and drives the two lifting rods 131 to ascend or descend, so that the process of supporting the ice ring in the crystallization concentration tank 10 is realized through the supporting plate 132 of the lifting belt Kong Binghuan, and the ice ring is convenient to take out.
The stirring device 14 comprises a stirring paddle 141, a sealing device 142 and a stirring motor 143. The stirring paddle 141 is disposed in the crystallization and concentration tank 10, and the top end thereof is mounted on the top of the crystallization and concentration tank 10 by the sealing device 142 and is connected with the power output end of the stirring motor 143.
The outer interlayer temperature probe 15 is disposed inside the outer interlayer 105, and is used for detecting and feeding back the temperature of the cold carrier II in the outer interlayer 105, i.e. the outer interlayer temperature.
The plurality of temperature recording probes 16 are arranged in the crystallization concentration tank 10 and are used for detecting and feeding back the temperature of the feed liquid in the tank. Specifically, the multiple sets of temperature recording probes 16 are uniformly distributed between the axial center and the inner wall in the crystallization concentration tank 10 at intervals, more preferably, the horizontal distance between every two adjacent sets of temperature recording probes 16 is 1-5 cm, and the distance between the outermost set of temperature recording probes 16 and the inner wall of the crystallization concentration tank 10 is 1-2 mm.
As shown in fig. 2, the cold carrier temperature control unit includes a cold carrier tank 20 containing a cold carrier ii, a temperature balance control box 21, a refrigeration compressor 22, a heat exchanger 23, a first low-temperature circulation pump 24, and a second low-temperature circulation pump 25.
The cold carrier tank 20, the temperature balance control box 21 and the outer interlayer 105 are connected through pipelines to form a circulation loop of cold carrier II circulation, which is called as 'outer circulation', wherein an inlet pipe of the cold carrier II is connected with the temperature balance control box 21, and an outlet valve 105b of the cold carrier II is connected with the cold carrier tank 20 through a pipeline. The first low-temperature circulating pump 24 is installed on a pipeline between the cold carrier tank 20 and the temperature balance control box 21 and is used for providing power for the cold carrier II in the external circulation, the feeding end of the first low-temperature circulating pump is connected with the cold carrier tank 20, and the discharging end of the first low-temperature circulating pump is connected with the temperature balance control box 21, so that the cold carrier II in the cold carrier tank 20 is pumped into the temperature balance control box 21.
The cold carrier tank 20 is internally provided with a cold carrier tank temperature probe 200 for detecting and feeding back the temperature of the cold carrier II in the tank, namely the cold carrier tank temperature. The temperature balance control box 21 is internally provided with a balance box temperature probe 210 and a multi-layer baffle, the balance box temperature probe 210 is used for detecting and feeding back the temperature of the cold carrier II in the box, namely the temperature of the temperature balance control box, and the cold carrier II in the input box forms turbulence when passing through the multi-layer baffle so as to realize rapid mixing with the original cold carrier II in the box.
The cold carrier tank 20 and the heat medium channel in the heat exchanger 23 are connected through a pipeline to form a circulation loop for circulating the cold carrier II, which is called as cooling internal circulation. The second low-temperature circulating pump 25 is arranged on a pipeline between the cold carrier tank 20 and the heat exchanger 23 and is used for providing power for the cold carrier II in the cooling internal circulation. The low-temperature refrigerant generated by the refrigeration compressor 22 is introduced into the refrigerant channel in the heat exchanger 23 to provide cold for the cold carrier II in the heat medium channel.
As shown in fig. 3, the parameter control and automatic recording unit includes an operating parameter panel 30, a controller 31, and an operation data recording storage 32. The operating parameter panel 30 and the operation data record reservoir 32 are electrically connected to the controller 31, respectively.
The operation parameter panel 30 is used for manually setting upper and lower limit values of the cold carrier tank temperature, the temperature balance control box temperature and the outer interlayer temperature according to the freezing concentration process.
The controller 31 is electrically connected to the outer sandwich temperature probe 15, the plurality of sets of temperature recording probes 16, the cold carrier tank temperature probe 200, the balancing tank temperature probe 210, the stirring motor 143, the temperature control solenoid valve 105a, the first low temperature circulation pump 24, the second low temperature circulation pump 25, and the refrigeration compressor 22, respectively.
The controller 31 is provided with an operation parameter management program, and controls the working states of the stirring motor 143, the temperature control electromagnetic valve 105a, the first low-temperature circulating pump 24, the second low-temperature circulating pump 25 and the refrigeration compressor 22 according to the temperature parameters fed back by the outer interlayer temperature probe 15, the plurality of groups of temperature recording probes 16, the cold carrier tank temperature probe 200 and the balance box temperature probe 210, so that the actual cold carrier tank temperature, the temperature balance control box temperature and the outer interlayer temperature reach the set ranges, and the feed liquid temperature in the crystallization concentration tank 10 is controlled in the freezing concentration process.
Specifically, the controller 31 controls the rotation speed of the stirring paddle 141 by controlling the rotation speed of the stirring motor 143; the controller 31 is electrically connected with the first low-temperature circulating pump 24 through a first frequency converter 240, and controls the power of the first low-temperature circulating pump 24 through controlling the first frequency converter 240, so as to control the flow rate of the external-circulation intercooled carrier II; the controller 31 is electrically connected to the second low-temperature circulation pump 25 through a second frequency converter 250, and controls the power of the second low-temperature circulation pump 25 through controlling the second frequency converter 250, so as to control the flow rate of the cooling medium ii in the cooling internal circulation.
The operational data recording reservoir 32 is used to record the operational data of the apparatus during the concentration freezing process. The operational data record store 32 may be connected to an external computer to export operational data for editing processes.
Example 2: freezing concentration method
The operation method for freeze concentration by using the progressive freeze concentration equipment with the double-sandwich structure comprises the following steps:
s1: and measuring the freezing point and supercooling point of the feed liquid to be concentrated.
S2: the temperature range of the first stage is set, and the crystallization and concentration tank 10 is cleaned, specifically by the following steps:
the equipment power is started and the operating parameter panel 30 is used to set the ranges of cold carrier tank temperature, temperature balance control box temperature and outer interlayer temperature, respectively. The lower limit value of the temperature of the cold carrier tank is the lowest, the upper limit value of the temperature of the cold carrier tank, the lower limit value of the temperature balance control box and the lower limit value of the outer interlayer temperature are all lower than the freezing point of the feed liquid to be concentrated, and the upper limit value of the temperature balance control box is the same as the upper limit value of the outer interlayer temperature and higher than the upper limit value of the temperature of the cold carrier tank. For example, the temperature of the temperature balance control box and the temperature of the outer interlayer can be set between 1 ℃ above and below the freezing point value of the feed liquid to be concentrated, and the upper limit value and the lower limit value of the three groups of temperatures are not more than 2-4 ℃ generally.
Fresh water is pumped into the crystallization concentration tank 10 by the heat preservation material tank 11 through the cryopump 12, the stirring device 14 is started to clean the tank for a plurality of times, the concentrate discharge valve 102 is opened to discharge the accumulated water, the concentrate discharge valve 102 and the circulation control valve 170 are closed, and the exhaust valve 103 is opened.
S3: the material liquid to be concentrated is fed, and the concrete steps are as follows:
the feed liquid inlet valve 101 is opened, the feed liquid to be concentrated is pumped into the crystallization concentration tank 10 in batches by using the cryopump 12 through the heat preservation feed cylinder 11 until the feed liquid level reaches the position of 2cm below the top end of the outer interlayer 105, and the feed liquid inlet valve 101 and the exhaust valve 103 are closed.
S4: the method comprises the following specific steps of:
the carrier I inlet valve 104a and the carrier I outlet valve 104b are opened, the carrier I is fed into the interior of the inner layer 104 by means of the cryopump 12 through the insulating cylinder 11 until it is completely filled, and the carrier I inlet valve 104a and the carrier I outlet valve 104b are closed.
S5: the cold carrier II is fed, and the external circulation is started, and the specific steps are as follows:
after filling the cold carrier tank 20 with the cold carrier II, opening the cold carrier II outlet valve 105b, starting the first low-temperature circulating pump 24, inputting the cold carrier II in the cold carrier tank 20 into the temperature balance control box 21, automatically opening the temperature control electromagnetic valve 105a, inputting the cold carrier II in the temperature balance control box 21 into the outer interlayer 105, filling the cold carrier II into the outer interlayer 105, and returning the cold carrier II into the cold carrier tank 20, so as to maintain the circulating flow of the cold carrier II among the cold carrier tank 20, the temperature balance control box 21 and the outer interlayer 105, and simultaneously, supplementing the cold carrier II into the cold carrier tank 20 through the outside, so that the volume of the cold carrier II in the tank is kept to 80% of the volume.
S6: starting cooling internal circulation, simultaneously keeping the operation of external circulation and cooling internal circulation, entering a first stage of freeze concentration, and specifically comprising the following steps:
the stirring device 14 is started, the stirring paddle 141 is rotated and adjusted to a high speed gear, the refrigeration compressor 22, the heat exchanger 23 and the second low-temperature circulating pump 25 are started again, the cold carrier II in the cold carrier tank 20 is input into the heat medium channel in the heat exchanger 23, the circulating flow of the cold carrier II between the cold carrier tank 20 and the heat medium channel in the heat exchanger 23 is maintained, the low-temperature refrigerant generated by the refrigeration compressor 22 is input into the refrigerant channel in the heat exchanger 23, when the temperature of the cold carrier tank is detected to be reduced to be within the range set in the step S2, the refrigeration compressor 22 automatically stops working, and when the temperature of the cold carrier tank is detected to be beyond the set upper limit value, the refrigeration compressor 22 is restarted. The temperature of the outer interlayer is steadily reduced by the internal and external circulation of the cold carrier II.
S7: setting the temperature range of the second stage, and entering the second stage of freeze concentration, wherein the method comprises the following specific steps:
when the temperature of the cold carrier tank, the temperature balance control box and the temperature of the outer interlayer are all detected to be within the range set in the step S2, and the difference between the temperature of the feed liquid in the crystallization concentration tank 10 and the freezing point of the feed liquid to be concentrated is detected to be 1-2 ℃, the ranges of the temperature of the cold carrier tank, the temperature balance control box and the temperature of the outer interlayer are reset by using the operation parameter panel 30. Wherein, the temperature of the temperature balance control box and the temperature of the outer interlayer are both set between 1 ℃ and 2 ℃ above and below the supercooling point value of the feed liquid to be concentrated, and the upper limit value of the temperature of the cold carrier tank is set to be 2 ℃ to 4 ℃ lower than the upper limit value of the temperature of the outer interlayer.
The second stage of freeze concentration is a critical period of time for the formation of pure ice crystals on the inner wall of the crystallization concentration tank 10, and no severe fluctuation of the feed liquid temperature can occur, and the temperature reduction on the inner side of the tank must be very stable so as to form granular ice crystals with high purity, rather than dendritic heterogeneous ice crystals.
S8: setting the temperature range of the third stage, entering the third stage of freeze concentration, and specifically comprising the following steps:
the stirring paddle 141 is kept in high-speed operation until obvious ice crystals are formed in the crystallization concentration tank 10, and the upper limit value and the lower limit value of the cold carrier tank temperature, the temperature balance control box temperature and the outer interlayer temperature set in the step S7 are respectively adjusted to be 4-6 ℃ by using the operation parameter panel 30.
S9: setting the temperature range of the fourth stage, entering the freezing and concentrating fourth stage, and collecting concentrated mother liquor, wherein the method comprises the following specific steps:
when the thickness of the ice ring formed on the inner wall of the crystallization concentration tank 10 reaches about 1cm, the ice layer forms obvious thermal resistance, the heat transfer of the liquid to the tank wall direction is affected, the stirring paddle 141 needs to be kept to operate at a high speed, meanwhile, the upper limit value and the lower limit value of the temperature of the cold carrier tank, the temperature balance control box and the temperature of the outer interlayer set in the step S8 are continuously adjusted by using the operation parameter panel 30, the upper limit value of the temperature of the outer interlayer set is kept to be lower than the detection temperature of the liquid in the crystallization concentration tank 10 by 4-8 ℃, at the moment, the thickening speed of the ice ring is reduced, but still the thickening is continuously carried out, the liquid is sampled from the concentrated liquid discharge valve 102 at regular time, the concentration of the sample liquid is detected, and after the concentration of the sample liquid reaches 2-4 times the concentration of the initial liquid, the concentrated liquid discharge valve 102 is opened to directly discharge and all the concentrated mother liquid is collected.
S10: and (3) ending freeze concentration, and collecting feed liquid with higher concentration, wherein the method comprises the following specific steps of:
the operation of the refrigeration compressor 22 is stopped, the ranges of the temperature balance control box temperature and the outer interlayer temperature are reset using the operation parameter panel 30, and the upper limit values of the temperature balance control box temperature and the outer interlayer temperature can be set to be higher than 0 c, and the circulation flow of the cold carrier ii among the cold carrier tank 20, the temperature balance control box 21 and the outer interlayer is maintained. The higher concentration liquid which is seeped out is preferably thawed and thawed by the ice ring in the crystallization concentration tank 10 through the concentrate discharge valve 102, and when the average concentration of the collected mixed liquid does not meet the concentration ratio requirement, the collection is stopped, and at the same time, the concentrate discharge valve 102 is closed, and the operation of the first low-temperature circulation pump 24 is stopped.
S11: thawing and precooling, and specifically comprises the following steps:
draining the carrier I in the inner interlayer 104, cleaning the inner interlayer 104 by clean water, then inputting the next batch of feed liquid to be concentrated into the inner interlayer 104 by using the cryopump 12, keeping circulating flow, thawing the outer wall of the ice ring in the crystallization concentration tank 10, and pre-cooling the next batch of feed liquid to be concentrated. Then the ice ring is lifted by the up-and-down sliding of the pneumatic lifting device 13, the tank top is opened, and the ice ring is taken out. The taken ice ring can be processed in a quick thawing mode outside the tank, and whether the subsequent recovery concentration is worth is evaluated according to the quality and the concentration of the thawing liquid.
S12: the operation data record storage 32 is connected to a computer via a router or a transmission line, and the freeze-concentrated operation data is exported for editing processing.
S13: the next batch of material liquid to be concentrated after precooling is pumped into the crystallization concentration tank 10, and the next round of freezing concentration is started.
Example 3: application of frozen concentration to fruit vinegar
The progressive freeze concentration equipment with the double-sandwich structure and the concentration method are applied to freeze concentration of clear and transparent food feed liquid, and specifically freeze concentration of fruit vinegar stock solution.
The fruit vinegar stock solution to be concentrated is clear transparent liquid, its weight is 50.6kg, the initial soluble solid content is 7.7%, total acid (calculated by acetic acid) is 1.87%, freezing point is-2.1 ℃, and supercooling point is-3.3 ℃.
The specific process operating parameters set in stages for freeze concentration and thawing are shown in table 1.
TABLE 1 Process operating parameters for stage setting of fruit vinegar freeze concentration
The first stage of freezing and concentrating in table 1 is the stage of lowering the temperature of the fruit vinegar to near the freezing point temperature; the second stage of freezing and concentrating is a stage of lowering the temperature of the fruit vinegar to be within the supercooling point range, and ice crystals are generated at the stage; the third stage of freeze concentration is a stage of forming a 1cm thick ice ring on the inner wall of the crystallization concentration tank by fruit vinegar; the fourth stage of freeze concentration is a stage of continuously thickening the fruit vinegar ice ring on the inner wall of the crystallization concentration tank to concentrate fruit vinegar, and after the stage is finished, collecting concentrated mother liquor with the maximum concentration; the thawing stage is to discharge concentrated mother liquor of fruit vinegar, and the concentrated fruit vinegar in the ice ring in the tank is infiltrated outwards, so that the fruit vinegar meeting the concentration requirement can be collected for the second time. And then draining the carrier I in the inner interlayer outside the crystallization concentration tank, cleaning, inputting the next batch of fruit vinegar to be concentrated into the inner interlayer, keeping circulating flow, thawing the outer wall of the ice ring in the crystallization concentration tank, and pre-cooling the next batch of fruit vinegar to be concentrated. Then the ice ring is slid up and down by the pneumatic lifting device, the tank top is opened, the ice ring is taken out, and the tank is quickly thawed outside by adopting a warm water bath.
In this embodiment, 4 sets of temperature recording probes are disposed in the crystallization concentration tank, for recording temperature changes of fruit vinegar during freeze concentration and thawing. Please refer to fig. 4, which is a graph showing temperature change of fruit vinegar at different positions in the crystallization and concentration tank during the freeze concentration and thawing process of the present embodiment; t in the figure 1 、T 2 、T 3 And T 4 And curves respectively representing fruit vinegar temperature curves recorded by four groups of temperature recording probes distributed between the inner wall of the tank and the axial center of the tank.
The specific freeze concentration results are shown in Table 2.
TABLE 2 comparison of fruit Vinegar concentration by freezing and comparison of stock solutions before concentration
The concentration ratio, concentration distribution coefficient and concentration ratio in table 2 were calculated by combining the concentrated fruit vinegar mother liquor discharged from the tank at the end of concentration and the thicker fruit vinegar discharged from the tank at the thawing stage and comparing the combined concentrated fruit vinegar mother liquor with the index value of the ice ring thawing liquid discharged from the tank.
Example 4: application of freeze concentration to citrus juice
The progressive freeze concentration equipment with the double-sandwich structure and the concentration method thereof are applied to freeze concentration of turbid food feed liquid, and specifically freeze concentration of citrus juice stock solution.
The stock citrus juice to be concentrated was a cloudy liquid weighing 36.7kg, having an initial soluble solids content of 8.3%, a freezing point of-2.3 ℃ and a supercooling point of-3.5 ℃.
The specific process operating parameters set in stages for freeze concentration and thawing are shown in table 3.
TABLE 3 Process operating parameters for stage-one freeze concentration stage-by-stage setting of citrus juice
Table 3 the first stage of freeze concentration is the stage of citrus juice temperature down to near freezing point temperature; the second stage of freezing concentration is a stage of reducing the temperature of the citrus juice to be within the range of the supercooling point, and ice crystals are generated in the stage; the third stage of freeze concentration is a stage of forming an ice ring with the thickness of about 1cm on the inner wall of the crystallization concentration tank; the fourth stage of freeze concentration is a stage of continuously thickening an ice ring of the citrus juice in the inner wall of a crystallization concentration tank to concentrate the citrus juice, and after the stage is finished, collecting concentrated mother liquor with the maximum concentration; and the thawing stage is to discharge the concentrated mother liquor of the citrus juice, then the thicker citrus juice in the ice ring in the tank is oozed, continuously collect the oozed thicker citrus juice meeting the first-stage concentration requirement, and combine the thicker citrus juice with the concentrated mother liquor collected before. And then draining the carrier I in the inner interlayer outside the crystallization concentration tank, cleaning, inputting the next batch of citrus juice to be concentrated into the inner interlayer, keeping circulating flow, thawing the outer wall of the ice ring in the crystallization concentration tank, and pre-cooling the next batch of citrus juice to be concentrated. Then the ice ring is slid up and down by the pneumatic lifting device, the tank top is opened, the ice ring is taken out, and the tank is quickly thawed outside by adopting a warm water bath.
In this embodiment, 4 sets of temperature recording probes are disposed in the crystallization concentration tank for recording temperature changes of the citrus juice during the freeze concentration and thawing process. Referring to fig. 5, a diagram showing temperature changes of citrus juice at different locations in a crystallization and concentration tank during freeze concentration and thawing according to the present embodiment; t in the figure 1 、T 2 、T 3 And T 4 Curves respectively representing the citrus juice temperatures recorded by four groups of temperature recording probes distributed between the inner wall of the tank and the axial center of the tankA degree curve.
The specific freeze concentration results are shown in Table 4.
TABLE 4 comparison of Primary freeze concentration effect of citrus juice with raw juice before concentration
The concentration ratio, concentration distribution coefficient and concentration ratio in table 4 were calculated by combining the concentrated citrus juice mother liquor discharged from the tank at the end of concentration with the thicker citrus juice discharged from the tank at the thawing stage and comparing the combined juice mother liquor with the index value of the ice ring thawing liquid discharged from the tank. It is noted that when the distribution coefficient of the feed liquid is relatively high, the solid content of the ice ring thawing liquid is relatively high, so that the ice ring thawing liquid is worth recycling, the collected multiple batches of entrained ice thawing liquid can be further recycled and concentrated.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (4)
1. A freeze concentration method, characterized in that: the method comprises the following steps:
(1) Measuring the freezing point and supercooling point of the feed liquid to be concentrated;
(2) Delivering the feed liquid to be concentrated into a crystallization concentration tank; the side wall of the crystallization concentration tank is of a double-interlayer structure with an inner interlayer and an outer interlayer, and stirring paddles are arranged in the tank;
(3) Filling the carrier I into the inner interlayer of the crystallization concentration tank; the carrier I is a food-grade carrier with heat transfer buffering characteristics;
(4) Inputting the cold carrier II into the outer interlayer of the crystallization concentration tank, keeping circulating flow, and simultaneously cooling the cold carrier II input into the outer interlayer by utilizing a refrigeration compressor and a heat exchanger; the cold carrier II is an anti-freezing cold carrier;
(5) The temperature of the feed liquid to be concentrated in the crystallization concentration tank is reduced in four stages by controlling the flow rate of the cold carrier II input into the outer interlayer, the working state of the refrigeration compressor and the rotating speed of the stirring paddle, and freezing concentration is carried out, so that an ice ring is formed in the tank; the first stage is to lower the temperature of the feed liquid to 1 ℃ above and below the freezing point value, the second stage is to lower the temperature of the feed liquid to 1 ℃ above and below the supercooling point value, the third stage is to lower the temperature of the feed liquid by 4-6 ℃ on the basis of the second stage, and the fourth stage is to continuously lower the temperature of the feed liquid on the basis of the third stage;
(6) When the feed liquid in the crystallization concentration tank reaches the target concentration, all the concentrated mother liquid in the tank is discharged and collected.
2. The freeze concentration process of claim 1 wherein: further comprising the step (7): and stopping the working of the refrigeration compressor, discharging and collecting the higher concentration feed liquid which is thawed and oozed by the ice ring in the crystallization concentration tank, and stopping collecting when the average concentration of the collected mixed feed liquid does not meet the concentration requirement.
3. The freeze concentration process of claim 2 wherein: further comprising the step (8): and (3) draining the carrier I in the inner interlayer of the crystallization concentration tank, cleaning the inner interlayer by using clear water, then inputting the next batch of feed liquid to be concentrated into the inner interlayer, keeping circulating flow, thawing the outer wall of an ice ring in the crystallization concentration tank, and pre-cooling the next batch of feed liquid to be concentrated.
4. A freeze concentration process according to claim 3 wherein: step (8) further comprises: after the next batch of concentrated feed liquid is precooled, an air-operated lifting device is used for supporting an ice ring in the crystallization concentration tank, the top of the tank is opened, and the ice ring is taken out; the pneumatic lifting device comprises two lifting rods, a belt Kong Binghuan supporting plate and an air cylinder, wherein the two lifting rods extend into the crystallization concentration tank, the bottom ends of the two lifting rods are fixedly connected with the belt Kong Binghuan supporting plate respectively, and the top ends of the two lifting rods are connected with the power output end of the air cylinder.
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CN109692495A (en) * | 2019-01-25 | 2019-04-30 | 中国石油化工股份有限公司 | A kind of crystallization kettle temperature control system and control method |
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