Freeze concentration method
By freezing, crushing, and fractionally extracting solutions from dilute solutions, the cryogenic concentration process is optimized, solving the problems of complex equipment, high cost, and low efficiency in existing technologies, and achieving highly efficient concentration and separation purification.
Patent Information
- Application Number
- PCT/CN2025/113833
- 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 complex, costly, and inefficient, while traditional multiple freeze-thaw cycles are time-consuming and inefficient.
The concentration process is optimized by freezing a dilute solution into a solid or a solid-liquid mixture, then crushing it, extracting the solution in segments, and repeating the steps as needed to increase the concentration. This is achieved by combining solid-liquid separation and crushing with heat transfer under different environments.
It improves the efficiency of freeze concentration and separation purification, simplifies the operation process, and facilitates applications in food, cosmetics, biomedicine, and environmental protection.
Smart Images

Figure PCTCN2025113833-FTAPPB-I100001 
Figure PCTCN2025113833-FTAPPB-I100002 
Figure PCTCN2025113833-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 state for 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, although this method is simple to operate, it takes a very long time and has low working efficiency, so it is rarely used in industrial freeze concentration. SUMMARY
[0004] To solve the problems existing in the prior art, the main purpose of the present application is to provide a freeze concentration method.
[0005] To solve the above technical problems, according to one aspect of the present application, the present application provides the following technical scheme:
[0006] A freeze concentration method, comprising the following steps:
[0007] S1, freeze the dilute solution to obtain a solid;
[0008] S2, crush the solid obtained by freezing, transfer heat to the crushed solid, and segmentally retain the solution to obtain solutions with different concentrations;
[0009] S3, the solution meeting the target concentration is transferred to the next link; the solution not meeting the target concentration is repeated steps S1-S2 to continue to increase the concentration of the solution.
[0010] A freeze concentration method, comprising the following steps:
[0011] S1, freeze the dilute solution to obtain a solid-liquid mixture;
[0012] S2, the solid-liquid mixture obtained by freezing is crushed and then subjected to solid-liquid separation, heat is transferred to the crushed ice obtained after the solid-liquid separation, and the solution is fractionally collected to obtain solutions with different concentrations;
[0013] S3, the solution meeting the target concentration is transferred to the next step, and the solution not meeting the target concentration is repeatedly subjected to steps S1-S2 to continuously increase the concentration of the solution.
[0014] A freezing concentration method, comprising the following steps:
[0015] S1, a dilute solution is frozen to obtain a solid-liquid mixture;
[0016] S2, the solid-liquid mixture is subjected to solid-liquid separation, the solid obtained after the solid-liquid separation is crushed to obtain crushed ice, heat is transferred to the obtained crushed ice, and the solution is fractionally collected to obtain solutions with different concentrations;
[0017] S3, the solution meeting the target concentration is transferred to the next step, and the solution not meeting the target concentration is repeatedly subjected to steps S1-S2 to continuously increase the concentration of the solution.
[0018] As a preferred scheme of the freezing concentration method, the crushing is performed in the freezing device.
[0019] As a preferred scheme of the freezing concentration method, the crushing is performed after the solid or the solid-liquid mixture is taken out of the freezing device.
[0020] As a preferred scheme of the freezing concentration method, the crushing process and the environment after the crushing are controlled to prevent the moisture in the air from freezing into ice on the surface of the solid after the crushing.
[0021] As a preferred scheme of the freezing concentration method, the solid-liquid separation is performed by natural outflow, negative pressure extraction or centrifugal separation.
[0022] To solve the above technical problems, according to another aspect of the present application, the present application provides the following technical scheme:
[0023] The freezing concentration method is applied in the fields of food, cosmetics, biological medicine, environmental protection treatment, etc.
[0024] The freezing concentration method is applied in the fields of milk, wine, fruit juice, coffee, tea, soy milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater desalination, wastewater treatment, etc.
[0025] The freezing concentration method is applied in the field of freezing concentration and separation and purification of heat-sensitive raw materials.
[0026] The application of the freezing concentration method to the freezing concentration and separation and purification of milk, wine, fruit juice, coffee, tea, soybean milk, soybean milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater desalination, wastewater treatment, etc.
[0027] The beneficial effects of the application are as follows:
[0028] The application provides a freezing concentration method. A dilute solution is frozen to obtain a solid or a solid-liquid mixture. The frozen solid or solid-liquid mixture is crushed or the solid-liquid mixture is separated first and then the solid is crushed. Heat is transferred to the crushed solid. The solution is fractionally retained to realize the freezing concentration of the dilute solution. The method improves the efficiency of freezing concentration and separation and purification, is simple to operate, and is convenient for application in the fields of food, cosmetics, biological medicine, environmental protection treatment, etc. DETAILED DESCRIPTION
[0029] The technical solutions in the embodiments will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.
[0030] The application provides a freezing concentration method, which breaks the traditional freezing concentration thinking, improves the efficiency of freezing concentration and separation and purification, is simple to operate, and is convenient for application in the fields of food, cosmetics, biological medicine, environmental protection treatment, etc.
[0031] The technical solutions of the application will be further described below in combination with specific embodiments.
[0032] Embodiment 1
[0033] 700 mL of thorny grape wine with an alcohol degree of 14.5%vol was filled into a rectangular container and then frozen into a solid at -58 ℃. The frozen solid was crushed and then dissolved at 23 ℃. The fractionally retained solution was obtained. The specific conditions of the fractionally retained solution are shown in Table 1.
[0034] Table 1: Specific conditions of the fractionally retained solution of Embodiment 1
[0035] Embodiment 2
[0036] 700 mL of thorny grape wine with an alcohol degree of 14.5%vol was filled into a rectangular container and then frozen into a solid at -58 ℃. The frozen solid was crushed and then dissolved at 23 ℃. The fractionally retained solution was obtained. The specific conditions of the fractionally retained solution are shown in Table 1.
[0037] Table 2: Specific conditions of the fractionally retained solution of Embodiment 2
[0038] Comparative Example 1
[0039] The difference from Example 1 is that the solid is not broken and the dissolution is carried out at 23℃.
[0040] The details of the fractionation of the solution are shown in Table 3.
[0041] Table 3 Details of the fractionation of the solution of Comparative Example 1
[0042] From the above examples and comparative examples, it can be seen that:
[0043] The alcohol degree of the first solution of Comparative Example 1 is 21.2%vol, which is increased by 46.2% compared with the raw dilute solution (the alcohol degree of the wild grape wine is 14.5%vol); the alcohol degree of Example 1 is 28.8%vol, which is increased by 98.6% compared with the raw dilute solution (the alcohol degree of the wild grape wine is 14.5%vol); the alcohol degree of Example 2 is 30.5%vol, which is increased by 110.3% compared with the raw dilute solution (the alcohol degree of the wild grape wine is 14.5%vol); from Example 1 and Comparative Example 1, it can be seen that the concentration efficiency of the dilute solution frozen into solid and then dissolved after being broken is much higher than that without being broken; from Example 1 and Example 2, it can be seen that the concentration efficiency achieved by dissolution at different temperatures is different, and the selection of a suitable dissolution heating temperature can improve the concentration efficiency.
[0044] The sum of the volume ratios of the first solution and the second solution of Example 1 and Comparative Example 1 is 27.4%, but the alcohol degree of Example 1 is increased to more than 24.5%vol, and the alcohol degree of Comparative Example 1 is only increased to more than 18.8%vol. Therefore, the concentration efficiency of the dilute solution frozen into solid and then dissolved after being broken is much higher than that without being broken. Moreover, the time consumption of Example 1 for taking the first solution is less than that of Comparative Example 1 for taking the first solution, and the solution concentration is higher.
[0045] The above only describes the preferred embodiments of the present application, and does not limit the patent scope 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 scope of the present application.
Claims
1. A freeze concentration method characterized by, The method comprises the following steps: S1, freezing the dilute solution to obtain a solid; S2, crushing the solid obtained by freezing, transferring heat to the crushed solid, and fractionally collecting the solution to obtain solutions with different concentrations; S3, transferring the solution with the target concentration to the next step; and repeating steps S1-S2 to continue to increase the concentration of the solution.
2. A freeze concentration method characterized by, The method comprises the following steps: S1, freezing the dilute solution to obtain a solid-liquid mixture; S2, crushing the solid-liquid mixture obtained by freezing, and then performing solid-liquid separation, transferring heat to the crushed ice, and fractionally collecting the solution to obtain solutions with different concentrations; S3, transferring the solution with the target concentration to the next step; and repeating steps S1-S2 to continue to increase the concentration of the solution.
3. A freeze concentration method characterized by, The method comprises the following steps: S1, freezing the dilute solution to obtain a solid-liquid mixture; S2, performing solid-liquid separation on the solid-liquid mixture, crushing the solid obtained by the solid-liquid separation to obtain crushed ice, transferring heat to the crushed ice, and fractionally collecting the solution to obtain solutions with different concentrations; S3, transferring the solution with the target concentration to the next step; and repeating steps S1-S2 to continue to increase the concentration of the solution.
4. The freeze concentration method according to any one of claims 1 to 3, characterized in that, The crushing is performed in the freezing device.
5. The freeze concentration method according to any one of claims 1 to 3, characterized in that, The crushing is performed after the solid or solid-liquid mixture is taken out of the freezing device.
6. The freeze concentration method according to any one of claims 1 to 3, characterized in that, The crushing process and the environment after crushing are controlled to prevent moisture in the air from freezing into ice on the surface of the crushed solid.
7. The freeze concentration method according to any one of claims 2 to 3, characterized in that, The solid-liquid separation is performed by natural flow, negative pressure extraction, or centrifugal separation.
8. Application of the freezing concentration method of any one of claims 1-7 in the fields of food, cosmetics, biomedicine, and environmental protection treatment.
9. Application of the freezing concentration method of any one of claims 1-7 in the fields of milk, wine, fruit juice, coffee, tea, soy milk, chemical liquid, Chinese herbal medicine liquid, plant extract, seawater desalination, and wastewater treatment.
Citation Information
Patent Citations
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