Freeze concentration method
By setting up a flow channel and transferring heat during the freezing process of dilute solutions, the problems of complex equipment and low efficiency in existing freeze concentration methods are solved, achieving efficient concentration and separation purification, which is applicable to multiple fields.
Patent Information
- Application Number
- PCT/CN2025/113834
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-08-12
- Filing Date
- 2025-08-11
- Publication Date
- 2026-02-19
AI Technical Summary
Existing freeze concentration methods are characterized by complex equipment, high cost, and low efficiency, while traditional heating and dissolving methods affect the concentration effect and efficiency.
When a dilute solution is frozen into a solid or a solid-liquid mixture, a flow channel is set up to transfer heat to it for dissolution and separation, and the concentration of the dilute solution is achieved through the flow channel.
It improves the efficiency of freeze concentration and separation purification, simplifies the operation, and is applicable to food, cosmetics, biopharmaceuticals, and environmental treatment.
Smart Images

Figure PCTCN2025113834-FTAPPB-I100001 
Figure PCTCN2025113834-FTAPPB-I100002 
Figure PCTCN2025113834-FTAPPB-I100003
Abstract
Description
Freeze concentration method TECHNICAL FIELD
[0001] The present application belongs to the technical field of freeze concentration, in particular to a freeze concentration method. BACKGROUND
[0002] The freeze concentration method in the prior art is a concentration technology realized by using the solid-liquid correlation of dilute solution and ice below the freezing point. There are mainly two ways: suspension crystallization freeze concentration method and gradual freeze concentration method. The principle of the suspension crystallization freeze concentration method is that when the dilute solution is frozen, the free small ice crystals suspended in the liquid are continuously removed, so that the concentration of the liquid is increased. The principle of the gradual freeze concentration method is that when the dilute solution is frozen, with the generation and growth of the ice layer on the cooling surface, the solute near the solid-liquid interface is excluded to the liquid phase side, resulting in the gradual increase of the mass concentration of the solute in the liquid phase. The existing freeze concentration method has complex equipment structure, high equipment cost and production cost, and low efficiency.
[0003] When the ice body is naturally dissolved, the solution with relatively high concentration will be dissolved first. By freezing the solution into solid multiple times and then dissolving it, the concentration of the dilute solution can be increased, which is a freeze concentration method through the natural dissolution of ice body. However, this method is simple to operate, but it takes a very long time and has low working efficiency, so it is rarely used in industrial freeze concentration.
[0004] In addition, some public information has devices and methods for heating and dissolving frozen materials to produce concentrated solutions, but the effect and efficiency of freeze concentration are not high due to the defects in the method. In the device and method disclosed in the patent application with publication number JP2004351383A, steam and hot gas are used to heat and dissolve the frozen materials. This method does not take into account the structural characteristics of the surface and interior of the frozen materials formed by freezing, which will affect the separation and outflow of the concentrated solution. In this method, the surface of the frozen materials and the ice layer adjacent to the container wall will be denser than the ice crystals inside the frozen materials, that is, the frozen materials are "surrounded" by a relatively dense ice layer; at the same time, the complex structure of the ice crystals inside the frozen materials will also hinder the separation and outflow of the concentrated solution inside. These factors affect the separation and outflow of the concentrated solution inside the frozen materials; thus, the effect and efficiency of freeze concentration of this method are affected and limited, which will affect the efficiency of industrial production and promotion. SUMMARY
[0005] To solve the problems in the prior art, the main purpose of the present application is to provide a freezing concentration method, which realizes the freezing concentration of a dilute solution by setting a flow guide channel on the solid or solid-liquid mixture obtained by freezing the dilute solution and transferring heat to the flow guide channel for dissolution and separation. The method improves the efficiency of freezing concentration and separation and purification.
[0006] To solve the above technical problems, according to one aspect of the present application, the present application provides the following technical solutions:
[0007] A freezing concentration method, comprising the following steps:
[0008] S1, freezing a dilute solution to obtain a solid or a solid-liquid mixture;
[0009] S2, setting a flow guide channel on the solid or solid-liquid mixture obtained by freezing;
[0010] S3, transferring heat to the solid or solid-liquid mixture provided with the flow guide channel, and segmentally taking out the solution to obtain solutions with different concentrations;
[0011] S4, transferring the solution meeting the target concentration to the next link, and repeating steps S1-S3 to continue to increase the concentration of the solution for the solution not meeting the target concentration.
[0012] As a preferred scheme of the freezing concentration method according to the present application, in the step S2, a plurality of flow guide channels are directly processed on the solid or solid-liquid mixture obtained by freezing; and the processing mode includes drilling, penetrating, inserting, piercing and the like.
[0013] As a preferred scheme of the freezing concentration method according to the present application, in the step S2, the flow guide channel is set by inserting a flow guide device on the solid or solid-liquid mixture obtained by freezing.
[0014] As a preferred scheme of the freezing concentration method according to the present application, in the step S2, the flow guide channel is set by destroying (crushing) the solid layer part in the outflow direction of the solution obtained by heating the solid or solid-liquid mixture.
[0015] As a preferred scheme of the freezing concentration method according to the present application, in the step S2, the flow guide channel is set by pre-setting a flow guide channel or a flow guide device with flow guide function during freezing.
[0016] As a preferred scheme of the freezing concentration method according to the present application, in the step S3, after the solid or solid-liquid mixture is heated, the solution is separated and flows out in the mode of natural outflow, negative pressure extraction or centrifugal separation.
[0017] As a preferred solution of the freeze concentration method, in step S3, the heat is transferred to the solid or solid-liquid mixture in the following manner:
[0018] The solid or solid-liquid mixture is naturally dissolved,
[0019] or the solid or solid-liquid mixture is directly heated,
[0020] or a heat source is arranged in a specific orientation inside or outside the solid or solid-liquid mixture.
[0021] As a preferred solution of the freeze concentration method, in step S3, the specific orientation is a directional area described as follows: from the cooling surface of the freeze concentration of the dilute solution into the solid or solid-liquid mixture, the specific orientation is the area away from the cooling surface in the direction of the solid or solid-liquid mixture. The area varies with the position of the cooling surface: it can be inside the solid or solid-liquid mixture, or outside. The heat source arranged in the specific orientation has the feature that when the heat is transferred to the solid or solid-liquid mixture, the heat is not first transferred to the solid layer with low solute content in the solid or solid-liquid mixture.
[0022] As a preferred solution of the freeze concentration method, in step S3, the shape of the heat source includes: point, line (column), surface (plate), and sphere.
[0023] To solve the above technical problems, according to another aspect of the present application, the present application provides the following technical solutions:
[0024] The freeze concentration method described above is applied in the fields of food, cosmetics, biological medicine, environmental protection treatment, etc.
[0025] The freeze concentration method described above is applied in the fields of milk, wine, fruit juice, coffee, tea, beverage, soy milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater purification, wastewater treatment, etc.
[0026] The freeze concentration method described above is applied in the field of freeze concentration and separation and purification of heat-sensitive raw materials.
[0027] The freeze concentration method described above is applied in the field of freeze concentration and separation and purification of milk, wine, fruit juice, coffee, tea, beverage, soy milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater purification, wastewater treatment, etc.
[0028] The present application has the following beneficial effects:
[0029] The application provides a freezing concentration method, which is based on the structural features of the solid or solid-liquid mixture formed when a dilute solution is frozen into a solid (ice body) or a solid-liquid mixture (ice body + concentrated solution), and the dilute solution is frozen and concentrated by setting a flow channel in the solid or solid-liquid mixture and transferring heat to the flow channel for dissolving and separating. The method improves the efficiency of freezing concentration and separation and purification, and is simple to operate and applicable in the fields of food, cosmetics, biological medicine and environmental protection treatment. DETAILED DESCRIPTION
[0030] The technical solutions in the embodiments will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the application, but not all the embodiments. Based on the embodiments in the application, all the other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.
[0031] The application provides a freezing concentration method, which breaks the traditional freezing concentration thought, improves the efficiency of freezing concentration and separation and purification, and is simple to operate and applicable in the fields of food, cosmetics, biological medicine and environmental protection treatment.
[0032] The technical solutions in the embodiments will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the application, but not all the embodiments. Based on the embodiments in the application, all the other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.
[0033] Embodiment 1
[0034] A freezing concentration method of a wild grape wine, 6L of wild grape wine with a wine degree of 23.56%vol is filled into a cylindrical container and then frozen into a solid at-40℃, a flow channel is set in the solid (5 flow holes are punctured), heating is performed from the outside of the solid, the dissolving temperature is 30℃ (referring to the temperature of a heat source), and the temperature of the separated solution is lower than 0℃ during the whole heating and dissolving process. The specific conditions of the separated solution are shown in Table 1.
[0035] Table 1 Specific conditions of the separated solution in Embodiment 1
[0036] Comparative Example 1
[0037] The difference from Embodiment 1 is that no flow channel is set in the solid.
[0038] The specific conditions of the separated solution are shown in Table 2.
[0039] Table 2 Specific conditions of the separated solution in Comparative Example 1
[0040] From the above embodiments and comparative examples, it can be seen that:
[0041] The first segment collection solution: when the volume of the wine liquid obtained by the comparative example 1 is 22%vol, the alcohol degree is 26.68%vol. When the volume of the wine liquid obtained by the example 1 is 22%vol, the alcohol degree is 34.5%vol. It can be seen that the alcohol degree of the example 1 with the flow channel is obviously improved, and the freezing concentration effect is obvious.
[0042] The second segment collection solution: the volume is the same, and the alcohol degree is not much different.
[0043] The third segment collection solution: the volume of the wine liquid obtained by the comparative example 1 is 16%vol, and the alcohol degree is 16.64%vol. The volume of the wine liquid obtained by the example 1 is 14.6%vol, and the alcohol degree is 11.27%vol. It can be seen that the solute (alcohol) of the solution in the segment with the flow channel (the example 1) is obviously less than that without the flow channel (the comparative example 1).
[0044] The fourth segment collection solution: the volume of the wine liquid obtained by the comparative example 1 is 12.5%vol, and the alcohol degree is 3.38%vol. The volume of the wine liquid obtained by the example 1 is 14.16%vol, and the alcohol degree is only 1.46%vol. It can be seen that the freezing concentration effect of the example 1 with the flow channel is obviously better than that of the comparative example 1 without the flow channel.
[0045] In summary, the present application is aimed at the structural characteristics of the solid or solid-liquid mixture formed by the freezing of the dilute solution into a solid (ice body) or a solid-liquid mixture (ice body + concentrated solution), and the dilute solution is frozen into a solid or solid-liquid mixture, the flow channel is set and the heat is transferred to the flow channel for dissolution and separation, so that the freezing concentration of the dilute solution is realized. The method improves the efficiency of freezing concentration and separation and purification, and is simple to operate and convenient to apply in the fields of food, cosmetics, biological medicine, environmental protection treatment and the like.
[0046] The above only describes the preferred embodiments of the present application, and does not limit the patent range of the present application, and any equivalent structural transformation made according to the content of the present application, or direct / indirect application in other related technical fields is included in the patent protection range of the present application.
Claims
1. A freeze concentration method, characterized by, It comprises the following steps: S1, freezing a dilute solution to obtain a solid or solid-liquid mixture; S2, setting a flow guide channel on the solid or solid-liquid mixture obtained by freezing; S3, transferring heat to the solid or solid-liquid mixture provided with the flow guide channel, and segmenting and retaining the solution to obtain solutions of different concentrations; S4, the solution meeting the target concentration is transferred to the next link; the solution not meeting the target concentration is repeated steps S1-S3 to continue to increase the concentration of the solution.
2. The freeze concentration method according to claim 1, characterized by, In step S2, the flow guide channel is set in the following ways: Directly processing a plurality of flow guide channels on the solid or solid-liquid mixture obtained by freezing; Or inserting a flow guide device on the solid or solid-liquid mixture obtained by freezing; Or destroying the solid layer part of the solution outflow direction of the solid or solid-liquid mixture after being heated; Or pre-setting a flow guide channel or a flow guide device with flow guide function during freezing.
3. The freeze concentration method according to claim 1, characterized by, In step S3, after the solid or solid-liquid mixture is heated, the solution separates and flows out in the following ways: natural outflow, negative pressure extraction or centrifugal separation.
4. The freeze concentration method according to claim 3, characterized by, In step S3, the heat is transferred to the solid or solid-liquid mixture provided with the flow guide channel in the following ways: The solid or solid-liquid mixture is naturally dissolved, Or directly heating the solid or solid-liquid mixture, Or setting a heat source in a specific orientation inside or outside the solid or solid-liquid mixture to heat.
5. The freeze concentration method according to claim 4, characterized in that, In step S3, the specific orientation is a description of a directional area: from the cooling surface when the dilute solution is frozen into a solid or solid-liquid mixture, the specific orientation is the area away from the cooling surface in the direction of the solid or solid-liquid mixture away from the cooling surface. The area is different with the position of the cooling surface: inside or outside the solid or solid-liquid mixture; the heat source set in the specific orientation, the heat transfer direction of the heat source is characterized by: when transferring heat to the solid or solid-liquid mixture, avoid the heat being transferred to the solid layer with low solute content in the solid or solid-liquid mixture first.
6. The freeze concentration method according to claim 4, characterized by, In step S3, the shape of the heat source includes: point, line, plane, sphere.
7. Application of the freeze concentration method of any one of claims 1-6 in the fields of food, cosmetics, biomedicine, and environmental protection treatment.
8. Application of the freeze concentration method of any one of claims 1-6 in the fields of milk, wine, fruit juice, coffee, tea, soy milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater purification, and wastewater treatment.
Citation Information
Patent Citations
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