CN117753043A - Low-temperature concentration method for reducing crystallization entrainment rate - Google Patents
Low-temperature concentration method for reducing crystallization entrainment rate Download PDFInfo
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Abstract
The present application relates to a low temperature concentration process to reduce the entrainment rate of crystals. According to the low-temperature concentration method for reducing the crystallization entrainment rate, small molecular gas is introduced at the stage before the phase transition of freezing concentration crystallization to form hydrate crystal nucleus or small crystals, so that the hydrate crystal nucleus or small crystals serve as seed crystals for freezing concentration, the supercooling degree of the freezing concentration crystallization can be reduced, and the freezing concentration is promoted. In the freezing concentration phase change stage, gas is continuously introduced, the nucleation point is increased while the heat transfer is enhanced, the crystallization is promoted to occur, more smaller ice crystals are formed, the generation of large ice crystals is effectively reduced, and the entrainment rate is reduced. By adopting the low-temperature concentration method for reducing the crystal entrainment rate, compared with single freezing concentration, the time is saved by more than 10%, the ice crystal entrainment rate is reduced by more than 10%, and the quality is improved by more than 15%.
Description
Technical Field
The application relates to the technology of concentrating liquid materials in the fields of biopharmaceuticals, foods, chemical synthesis and the like, in particular to a low-temperature concentration method for reducing the entrainment rate of crystals.
Background
Concentration is an important means commonly used in the fields of biopharmaceuticals, food processing, chemical synthesis and the like, concentrated solution is widely circulated as a semi-finished product or product, and a high-efficiency, high-quality and low-cost concentration means is always an urgent need of the concentration industry.
Traditional liquid concentration modes include membrane concentration, evaporative concentration and freeze concentration. The freezing concentration is a concentration method which uses the solid-liquid phase balance principle between ice and water solution to cool down the dilute solution until part of water in the solution is frozen into ice and separates ice crystals, and is suitable for the fields of liquid food concentration, concentration and separation of heat sensitive medicines and biological products, wastewater treatment, sea water desalination and the like. The method is mainly characterized by comprising four processes of seed crystal generation, crystal growth, solid-liquid separation and crystal washing, wherein the number, size and shape of ice crystals are key to the whole technology. Prevention of micro ice crystal adhering liquid in the process of seed crystal, avoidance of secondary nucleation in the process of ice crystal growth and inhibition of ice crystal growth speed are main factors affecting the concentration quality, namely ideal ice crystal is required to be obtained. The disordered large ice crystals have high entrainment rate, are easy to cause solute loss and nutrient loss, require complex crystal washing steps, and cause irreversible loss of solute to a certain extent in the crystal washing process, thereby finally obviously affecting the quality of the concentrated juice.
The hydrate method concentration is a concentration method that guest gas water molecules and host water molecules in solution form cage-shaped structural substances similar to ice crystals under certain pressure and temperature, and concentrated solution is obtained after solid-liquid separation; the formation of hydrate includes two stages of crystal nucleation and crystal growth, in the early stage of nucleation, gas molecules enter the solution, gas bubbles gradually become smaller along with the progress of gas-liquid mass transfer, gas molecules enter the cage-shaped pore structure formed by main water molecules gradually, nucleation occurs, main guest molecules are mutually related through Van der Waals force, stable cages are formed continuously in a gathering mode, and finally crystallization is completed.
The hydrate method concentration has similar effect with the currently recognized relatively optimal freeze concentration, similar problems of crystal entrainment solute loss exist, solution solute is easy to be entrained or even embedded in the process of crystal formation (forming cage-shaped structural substances), and the hydrate entrainment rate is one of main factors limiting popularization and application. But compared with freeze concentration, the method does not need subzero low temperature and has low energy consumption. Therefore, the formation speed, shape and size of the hydrate crystal are effectively regulated and controlled, and stable, more and pure hydrate crystals are obtained, so that concentrated solution with high concentration rate and low entrainment rate is obtained, and the method is an important guarantee for promoting the technical popularization of the liquid food concentrated by a hydrate method.
Thus, the above concentration techniques have some drawbacks, mainly represented by:
(1) The concentration efficiency of evaporation concentration is high, but the heat sensitive functional and nutritional components in the materials are seriously damaged.
(2) The freeze concentration has relatively high concentration quality, but the low-temperature freezing condition requires high concentration energy consumption, long time and high entrainment rate, and the freeze concentration also needs crystal washing operation, and in addition, sterilization treatment is still needed to store the finished concentrated juice for a long time, so that the application of the freeze concentration is relatively limited.
(3) The hydrate is concentrated, the entrainment rate is high, the sterilization effect on materials is limited, the phenomenon of sublethal of microorganisms occurs, and the materials can be stored for a long time only by auxiliary sterilization treatment.
Disclosure of Invention
Based on this, the present application provides a low temperature concentration process that reduces the entrainment rate of crystals. The method combines gas hydrate concentration and freeze concentration by optimizing the time, quantity and distribution of gas introduction so as to improve the crystallization process and reduce solute entrainment, thereby improving the purity and nutrition quality of the product.
The application provides a low-temperature concentration method for reducing crystallization entrainment rate, which comprises the following steps:
s100, pre-cooling the liquid material, and controlling the temperature of an inner cavity of a concentration processor to be consistent with the pre-cooling temperature of the liquid material;
s200, feeding the precooled liquid material into an inner cavity of the concentration processor;
s300, inputting small molecular gas into the inner cavity of the concentration processor, stirring the liquid material, and regulating and controlling the inner cavity pressure of the concentration processor to be a first pressure;
s400, continuously conveying the precooled liquid material into the inner cavity of the concentration processor, and reducing the temperature of the inner cavity of the concentration processor;
s500, continuously inputting small molecular gas into the inner cavity of the concentration processor, regulating and controlling the pressure of the inner cavity of the concentration processor to a second pressure, and increasing the stirring speed, wherein the second pressure is lower than the first pressure;
and S600, when the liquid material in the inner cavity of the concentration processor reaches the target concentration, discharging the liquid material from the inner cavity of the concentration processor, collecting all concentrated mother liquor, and taking out the annular ice crystals at the upper layer.
In one embodiment, in step S100, the liquid material is pre-cooled to a temperature of 0.5-8 ℃; in step S4O0, the temperature of the inner cavity of the concentration processor is reduced to-1 to-12 ℃.
In one embodiment, in step S100, when the precooled liquid material is sent into the inner cavity of the concentration processor, the volume of the liquid material is controlled to be 1/4-2/5 of the total volume of the inner cavity of the concentration processor; in step S4O0, continuously conveying the precooled liquid material into the inner cavity of the concentration processor, and controlling the volume of the liquid material to be 1/2-4/5 of the total volume of the inner cavity of the concentration processor.
In one embodiment, in step S300, stirring is achieved by providing a stirrer in the inner cavity of the concentration processor, wherein the stirring speed of the stirrer is set to 500-1500rpm/min; in the step S5O0, small molecular gas is continuously input in the cooling process, and the stirring speed of the stirrer is increased to 1500-2500 rpm/min.
In one embodiment, in step S300, the internal cavity pressure of the concentration processor is regulated to 3-10MPa; in the step S5O0, the inner cavity pressure of the concentration processor is regulated and controlled to be 2-5MPa.
In one embodiment, the small molecule gas is at least one of: CO2, C2H4, CH4, N2.
Compared with the prior art, the low-temperature concentration method for reducing the crystallization entrainment rate has the following advantages:
in the phase transition stage of freezing concentration crystallization, small molecular gas is introduced to form hydrate crystal nucleus or small crystal to serve as seed crystal for freezing concentration, so that the supercooling degree of freezing concentration crystallization can be reduced, and the occurrence of freezing concentration is promoted.
In the freezing concentration phase change stage, gas is continuously introduced, the nucleation point is increased while the heat transfer is enhanced, the crystallization is promoted to occur, more smaller ice crystals are formed, the generation of large ice crystals is effectively reduced, and the entrainment rate is reduced.
By adopting the low-temperature concentration method for reducing the crystal entrainment rate, compared with single freezing concentration, the time is saved by more than 10%, the ice crystal entrainment rate is reduced by more than 10%, and the quality is improved by more than 15%.
Drawings
FIG. 1 is a schematic diagram showing steps of a low temperature concentration method for reducing crystallization entrainment rate according to an embodiment of the present application;
FIG. 2 is a schematic structural diagram of an apparatus for implementing a low-temperature concentration method for reducing the entrainment rate of crystals according to an embodiment of the present application.
Reference numerals illustrate:
10. a concentrating processor; 110. an inner cavity; 111. a stirrer; 112. a pressure sensor; 113. a temperature sensor; 114. a liquid level sensor; 115. a concentration sensor; 116. a camera; 117. an air valve; 20. a feed tank; 30. a material transfer pump; 40. a gas delivery pump; 50. a collector.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings, wherein like reference numerals in the various drawings refer to the same or similar elements unless otherwise specified. Moreover, the embodiments described in the following exemplary examples are not intended to limit the present invention, and structural, methodological, or functional modifications made by one of ordinary skill in the art based on these embodiments are included within the scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms first, second, third, etc. may be used herein to describe various information, these information should not be limited by these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the invention. The word "if" as used herein may be interpreted as "at … …" or "at … …" or "responsive to a determination", depending on the context.
Aiming at the technical problems mentioned in the background art, the embodiment of the application provides a low-temperature concentration method for reducing the crystallization entrainment rate, which combines gas hydrate concentration and freeze concentration by optimizing the time, quantity and distribution of gas introduction so as to improve the crystallization process, reduce solute entrainment, reduce the crystallization entrainment rate to the greatest extent, ensure the concentration rate and the concentration quality, and further improve the purity and the nutrition quality of the product.
Hereinafter, a method for low-temperature concentration for reducing the crystallization entrainment rate according to the embodiments of the present invention will be described in more detail, but the invention is not limited thereto.
Embodiments of the present application provide a low temperature concentration method for reducing crystallization entrainment rate, which may be applied to the fields of biopharmaceuticals, foods, chemical synthesis and the like, but is not limited thereto.
As shown in fig. 1, fig. 1 is a flowchart illustrating a method for low-temperature concentration for reducing the entrainment rate of crystals according to an exemplary embodiment of the present application, where the method for low-temperature concentration for reducing the entrainment rate of crystals according to the embodiment of the present application includes the following steps:
s100, pre-cooling the liquid material, and controlling the temperature of the inner cavity of the concentration processor to be consistent with the pre-cooling temperature of the liquid material;
s200, feeding the precooled liquid material into an inner cavity of the concentration processor;
s300, inputting small molecular gas into the inner cavity of the concentration processor, stirring the liquid material, and regulating and controlling the inner cavity pressure of the concentration processor to be a first pressure;
s400, continuously conveying the precooled liquid material into the inner cavity of the concentration processor, and reducing the temperature of the inner cavity of the concentration processor;
s500, continuously inputting small molecular gas into the inner cavity of the concentration processor, regulating and controlling the pressure of the inner cavity of the concentration processor to a second pressure, and increasing the stirring speed, wherein the second pressure is lower than the first pressure;
and S600, when the liquid material in the inner cavity of the concentration processor reaches the target concentration, discharging the liquid material from the inner cavity of the concentration processor, collecting all concentrated mother liquor, and taking out the annular ice crystals at the upper layer.
The liquid material can be an intermediate material or a final material produced in the fields of biopharmaceuticals, food processing, chemical synthesis and the like, and parameters such as specific temperature, pressure, stirring speed and the like in the steps can be specifically set according to different liquid materials.
In a preferred example, in step S100, the liquid material is pre-cooled to a temperature of 0.5-8deg.C. In step S100, when the precooled liquid material is sent into the inner cavity of the concentration processor, the volume of the liquid material is controlled to be 1/4-2/5 of the total volume of the inner cavity of the concentration processor. In step S300, the small molecule gas is used to react with water molecules to form hydrate crystals, serving as seed crystals for ice crystals. Preferably, the small molecular gas in the present application may be CO2, C2H4, CH4, N2, or the like, or may be other small molecular gas capable of forming hydrates. In step S300, stirring is preferably achieved by providing a stirrer in the inner cavity of the concentration processor, the rotational speed is set to 500-1500rpm/min, and the inner cavity pressure of the concentration processor is regulated to 3-10MPa, that is, the range of the first pressure is 3-10MPa. In step S400, the real-time phase change curve and the temperature curve of the liquid material in the inner cavity of the concentration processor may be monitored, and the on-line camera may observe, so as to monitor that the liquid material is phase-changed to form a small seed crystal, thereby continuously conveying the precooled liquid material into the inner cavity of the concentration processor, wherein a temperature sensor may be disposed in the inner cavity of the concentration processor to monitor the temperature curve, a pressure sensor may be disposed to monitor the pressure, and the real-time phase change curve may be obtained through the temperature and pressure change judgment.
In step S4O0, preferably, the volume of the liquid material is controlled to be 1/2-4/5 of the total volume of the inner cavity, and the temperature of the inner cavity of the concentration processor is reduced to minus 1 ℃ to minus 12 ℃.
In the step S5O0, small molecular gas is continuously input in the cooling process, the inner cavity pressure of the concentration processor is regulated and controlled to be 2-5MPa, and the stirring speed of the stirrer is increased to be 1500-2500 rpm/min. In step S6O0, a concentration sensor may be disposed in the inner cavity of the concentration processor to monitor the concentration of the liquid material in real time.
Compared with the prior art, the low-temperature concentration method for reducing the crystallization entrainment rate has the following advantages:
(1) In the phase transition stage of freezing concentration crystallization, small molecular gas is introduced to form hydrate crystal nucleus or small crystal to serve as seed crystal for freezing concentration, so that the supercooling degree of freezing concentration crystallization can be reduced, and the occurrence of freezing concentration is promoted.
(2) In the freezing concentration phase change stage, gas is continuously introduced, the nucleation point is increased while the heat transfer is enhanced, the crystallization is promoted to occur, more smaller ice crystals are formed, the generation of large ice crystals is effectively reduced, and the entrainment rate is reduced.
By adopting the low-temperature concentration method for reducing the crystal entrainment rate, compared with single freezing concentration, the time is saved by more than 10%, the ice crystal entrainment rate is reduced by more than 10%, and the quality is improved by more than 15%.
As shown in fig. 2, fig. 2 is an apparatus for implementing a cryoconcentration method for reducing the entrainment rate of crystals according to an embodiment of the present application, which includes a concentration processor 10, a feed tank 20, a material transfer pump 30, a gas transfer pump 40 and a collector 50 according to the conventional art, wherein the concentration processor 10 has an inner cavity 110, and the concentration processor can adjust the temperature and pressure of the inner cavity. The inner cavity 110 is provided with a stirrer 111, a pressure sensor 112, a temperature sensor 113, a liquid level sensor 114, a concentration sensor 115 and a camera 116, the concentration processor 10 is also provided with an exhaust pipeline which is communicated with the inner cavity 110 and the outside, and the exhaust pipeline is provided with an air valve 117. Which are used to detect the pressure, temperature, level and concentration of the liquid material in the chamber 110, respectively. And a real-time phase change curve is obtained through temperature and pressure changes.
Specifically, the liquid material may be pre-cooled in a refrigerator, the feed tank 20 is used for transferring and storing the pre-cooled liquid material, the material transfer pump 30 is used for transferring the liquid material in the feed tank 20 to the inner cavity 110, the gas transfer pump 40 is used for inputting small molecular gas into the inner cavity 110, the collector 50 is used for collecting all concentrated mother liquor discharged from the inner cavity 110, and the upper annular ice crystal is taken out. In a preferred example, the feed tank 20 and the internal cavity of the concentrating processor may be cyclically cooled by providing a condensing circulation system to ensure that the temperature of both are consistent with the temperature of the pre-cooled liquid material.
In some embodiments, a controller is also included. The control device can be a singlechip, a PLC, a computer and the like, and the operation of the equipment is controlled by a controller.
A cryoconcentration process for reducing the entrainment of crystals in the examples of the present application is described in detail below by way of several specific examples. The specific conditions are not noted in the examples of the present application, and are performed according to conventional conditions or conditions suggested by the manufacturer. The raw materials, reagents, etc. used, which are not noted to the manufacturer, are conventional products commercially available.
Example 1
Peeling and juicing fructus Citri Limoniae with maturity of 8-9 to obtain fructus Citri Limoniae juice with solid content of 8obrix, and pre-cooling to 5deg.C in a refrigerator. And (3) opening a condensation circulation system to cool so that the temperature of the inner cavities of the feeding tank and the concentration processor is consistent with the temperature of the pre-cooling of the lemon juice. Pumping 2.5L of precooled lemon juice from a feeding tank into the inner cavity of a concentration processor, wherein the volume of the lemon juice liquid is 1/4 of the volume of the inner cavity, introducing CO2, opening a stirring device, setting the stirring speed to be 500rpm/min, and closing an air valve after the pressure reaches 3 MPa; after monitoring that the phase change occurs, the air valve is opened for air release, 2.5L of precooled lemon juice is continuously added, the temperature of the inner cavity of the concentration processor is reduced to minus 1 ℃, CO2 gas is continuously input until the pressure of the concentration processor reaches 2MPa, the air valve is closed, the stirring speed is increased to 1500rpm/min, when the concentration of the concentrated juice in the inner cavity is monitored to reach 26obrix, the concentrated juice is discharged from a discharge hole at the lower end, and annular ice crystals are taken out from the upper end. The entrainment rate of the obtained ice crystals is 1.5%, which is reduced by 10% compared with single freezing concentration, the phase change time of concentration is shortened by 10% without crystal washing step, and the influence of vitamin C and the like in the concentrated juice is respectively improved by 5% and more than 10% compared with the influence of independent freezing concentration and gas hydrate concentration.
Example 2
Peeling pineapple with maturity of 8-9, squeezing to obtain solid content of 11obrix, and pre-cooling to 3deg.C in a refrigerator. And (3) opening a condensation circulation system to cool so that the temperature of the inner cavities of the feeding tank and the concentration processor is consistent with the pre-cooling temperature of the pineapple juice. Pumping 4L of pre-cooled pineapple juice into the inner cavity of a concentration processor from a feeding tank, wherein the volume of the pineapple juice is 2/5 of the volume of the inner cavity, introducing CO2, opening a stirring device, setting the stirring speed to 1000rpm/min, and closing an air valve after the pressure reaches 4 MPa; after the phase change is monitored, an air valve is opened for air release, pre-cooling pineapple juice 4L is continuously added, the temperature of the inner cavity of a concentration processor is reduced to-4 ℃, CO2 gas is continuously input until the pressure of the inner cavity of the concentration processor reaches 3MPa, the air valve is closed, the stirring speed is increased to 2000rpm/min, when the concentration of the concentrated juice in the inner cavity of the concentration processor reaches 33obrix, the concentrated juice is discharged from a discharge hole at the lower end, and annular ice crystals are taken out from the upper end. The entrainment rate of the obtained ice crystals is 2.5%, which is reduced by 15% compared with single freezing concentration, the crystal washing step is not needed, the concentrating phase change time is shortened by 12%, and the influence of proteins and the like in the concentrated juice is respectively improved by 8% and 12% or more compared with the independent freezing concentration and gas hydrate concentration.
Example 3
Removing shells of litchi with maturity of 8-9, pulping, squeezing to obtain litchi juice with solid content of 14obrix, and pre-cooling in cold storage to 0.5 ℃. And (3) opening a condensation circulation system to cool so that the temperature of the inner cavities of the feeding tank and the concentration processor is consistent with the pre-cooling temperature of the litchi juice. Pumping 3L of precooled litchi juice from a feed tank into an inner cavity of a concentration processor, wherein the liquid is 3/10 of the volume of the inner cavity, introducing CO2, opening a stirring device, setting the stirring speed to 1500rpm/min, and closing an air valve after the pressure reaches 6 MPa; after 20min of treatment, the air valve is opened for air release, then 4L of precooled juice is continuously added, the temperature of the inner cavity of the concentration processor is reduced to minus 6 ℃, CO2 gas is continuously input until the pressure of the inner cavity of the concentration processor reaches 4MPa, the air valve is closed, the stirring speed is increased to 2500rpm/min, when the concentration of the concentrated juice in the inner cavity of the concentration processor reaches 35obrix, the concentrated juice is discharged from a discharge hole at the lower end, and the annular ice crystals are taken out from the upper end. The entrainment rate of the obtained ice crystals is 2%, which is reduced by 14% compared with single freezing concentration, the crystal washing step is not needed, the concentrating phase change time is shortened by 14%, and the influence of proteins and the like in the concentrated juice is respectively improved by 7%, 13% or more than that of the single freezing concentration and the gas hydrate concentration.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples only represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the claims. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (6)
1. A low temperature concentration method for reducing crystallization entrainment rate, which is characterized by comprising the following steps:
s100, pre-cooling the liquid material, and controlling the temperature of an inner cavity of a concentration processor to be consistent with the pre-cooling temperature of the liquid material;
s200, feeding the precooled liquid material into an inner cavity of the concentration processor;
s300, inputting small molecular gas into the inner cavity of the concentration processor, stirring the liquid material, and regulating and controlling the inner cavity pressure of the concentration processor to be a first pressure;
s400, continuously conveying the precooled liquid material into the inner cavity of the concentration processor, and reducing the temperature of the inner cavity of the concentration processor;
s500, continuously inputting small molecular gas into the inner cavity of the concentration processor, regulating and controlling the pressure of the inner cavity of the concentration processor to a second pressure, and increasing the stirring speed, wherein the second pressure is lower than the first pressure;
and S600, when the liquid material in the inner cavity of the concentration processor reaches the target concentration, discharging the liquid material from the inner cavity of the concentration processor, collecting all concentrated mother liquor, and taking out the annular ice crystals at the upper layer.
2. The low temperature concentration process for reducing the entrainment of crystals as set forth in claim 1 wherein:
in the step S100, the liquid material is pre-cooled to a temperature of 0.5-8 ℃; in step S4O0, the temperature of the inner cavity of the concentration processor is reduced to-1 to-12 ℃.
3. The low temperature concentration process for reducing the entrainment of crystals as set forth in claim 2 wherein:
in step S100, when the precooled liquid material is sent into the inner cavity of the concentration processor, controlling the volume of the liquid material to be 1/4-2/5 of the total volume of the inner cavity of the concentration processor; in step S4O0, continuously conveying the precooled liquid material into the inner cavity of the concentration processor, and controlling the volume of the liquid material to be 1/2-4/5 of the total volume of the inner cavity of the concentration processor.
4. A low temperature concentration process for reducing crystallization entrainment according to claim 3, characterized in that:
in step S300, stirring is realized by arranging a stirrer in the inner cavity of the concentration processor, wherein the stirring speed of the stirrer is set to be 500-1500rpm/min; in the step S5O0, small molecular gas is continuously input in the cooling process, and the stirring speed of the stirrer is increased to 1500-2500 rpm/min.
5. The method for low-temperature concentration for reducing the entrainment rate of crystals as set forth in claim 4, wherein:
in the step S300, regulating and controlling the inner cavity pressure of the concentration processor to 3-10MPa; in the step S5O0, the inner cavity pressure of the concentration processor is regulated and controlled to be 2-5MPa.
6. The low temperature concentration process for reducing the entrainment of crystals as set forth in claim 1 wherein:
the small molecule gas is at least one of the following: CO2, C2H4, CH4, N2.
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