CN112108086B - Directional solidification segregation device and method for colloidal particle system - Google Patents
Directional solidification segregation device and method for colloidal particle system Download PDFInfo
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- CN112108086B CN112108086B CN202011018047.2A CN202011018047A CN112108086B CN 112108086 B CN112108086 B CN 112108086B CN 202011018047 A CN202011018047 A CN 202011018047A CN 112108086 B CN112108086 B CN 112108086B
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Abstract
The invention relates to a directional solidification segregation device of a colloid particle system, which comprises a heat-insulating pipe and a low-temperature bottom plate arranged at the bottom of the heat-insulating pipe, wherein a solidification cabin is formed in the heat-insulating pipe, the solidification cabin is provided with a stock solution inlet, a purified solvent outlet, a concentrated product outlet and a pressure regulating device, and a rotor and a grid internally provided with nucleating agent crystal particles are arranged in the solidification cabin. Compared with the prior art, the invention limits the space of the nucleating agent crystal particles by adopting the mesh grid, thereby avoiding the pollution to a stock solution system while ensuring the nucleating position; reverse rotor produces the vortex, and the high efficiency is carried the granule of segregation to inside the liquid phase district, avoids leading to macrosegregation to lose efficacy because the granule piles up and causes the fracture of solidification front. The invention is suitable for the separation and purification process of complex component stock solution in the fields of metallurgical industry, biomedicine, food engineering and the like.
Description
Technical Field
The invention relates to the technical field of processing and preparation, in particular to a directional solidification segregation device and a directional solidification segregation method for a colloid particle system.
Background
Colloidal particle systems generally refer to a complex system consisting of two phases of a liquid solvent matrix and suspended particles (solid particles, bubbles, droplets, macromolecules and ions). In many industrial application settings, separation of liquid solvents and suspended particles is required. As solvent molecules are transformed from a disordered state to a long-range order during solidification crystallization, solid particles suspended therein or foreign substances (in molecular or ionic form) dissolved therein are removed from the solidification interface by hindering lattice matching, i.e., solidification segregation.
The solidification segregation is carried out in a low-temperature environment in the whole process, and other physical fields are not required to be applied, so that the method is particularly suitable for separating and purifying liquid raw materials in the fields of biological medicine and food engineering. However, conventional solidification segregation has several distinct disadvantages:
1. the position and the appearance of the solidification front are random, so that a solidification phase and a residual liquid phase are mixed, and the segregation efficiency is low;
2. the supercooling degree required by spontaneous solidification nucleation is large, the energy consumption is high, and the segregation efficiency can be obviously reduced by the rapid expansion of dendritic crystals under the large supercooling degree;
3. the addition of the nucleating agent can cause pollution to stock solution, and the spatial distribution of the nucleating agent, namely the position where a subsequent solidified phase appears, cannot be controlled;
4. high-concentration particles (containing solute molecules/ions) are accumulated on the solidification front and cannot be dispersed to a liquid phase in time, so that the solidification front is broken, and segregation failure is caused.
Disclosure of Invention
The present invention aims to overcome the defects of the prior art and provide a directional solidification segregation apparatus and method for a colloidal particle system.
The purpose of the invention can be realized by the following technical scheme:
the directional solidification segregation device of the colloid particle system comprises a heat insulation pipe and a low-temperature bottom plate arranged at the bottom of the heat insulation pipe, wherein a solidification cabin is formed inside the heat insulation pipe, the solidification cabin is provided with a stock solution inlet, a purified solvent outlet, a concentrated product outlet and a pressure regulating device, and a rotor and a grid internally provided with nucleating agent crystal particles are arranged in the solidification cabin.
Preferably, the rotor is provided with an even number, floats or is fixed on the upper part of the solidification cabin, and is symmetrically arranged along the radial direction.
Preferably, the rotor is a floating electromagnetic rotor or a position-defined mechanical rotor.
Preferably, the heat insulating pipe is a metal pipe, a glass pipe coated with a porous material layer, or a polymer pipe.
Preferably, the heat insulation pipe is provided with a scale bar.
Preferably, the low-temperature soleplate is made of heat-conducting metal or semiconductor.
Preferably, the size of the mesh grid is smaller than the inner diameter of the solidification cabin, and the mesh grid is fixed at the bottom of the solidification cabin close to the edge.
The directional solidification segregation method of the colloid particle system adopts the directional solidification segregation device, and comprises the following steps:
s1, injecting the colloidal particle stock solution into the solidification cabin, and adjusting the temperature of the low-temperature bottom plate to be lower than the solidification point of the equilibrium state after the liquid level is stable;
s2, generating a vortex flow field in the liquid phase region through a rotor reversely rotating near the gas-liquid interface to assist the transportation of segregation particles;
s3, after the stock solution with a certain proportion is solidified, extracting the concentrated suspension;
s4, melting the solidified phase by heating the low-temperature soleplate, and extracting the purified matrix solvent.
Preferably, the matrix solvent of the colloidal particle stock solution is water, a single organic solvent, a mixed organic solvent or a liquid metal.
Preferably, the colloidal particles of the colloidal particle stock solution are solid particles, microbubbles, micro-droplets, soluble macromolecules or ions. Compared with the prior art, the invention has the following beneficial effects:
1. by establishing a unidirectional temperature gradient and limiting the positions of crystal particles of the nucleating agent, the purity of the stock solution is guaranteed, the solidification nucleation position and the frontal surface propelling direction are controlled, the separation and purification efficiency is improved, and the method is suitable for separation and purification processes of complex component stock solutions in a plurality of fields such as metallurgical industry, biological medicine, food engineering and the like.
2. A vortex rotational flow field is established in a liquid phase region through an electromagnetic/mechanical rotor, particle diffusion is promoted, interface collapse and segregation failure caused by accumulation of particles at a solidification front are avoided, and the method is particularly suitable for treatment of large particles and high-concentration stock solution samples.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is a schematic view of the apparatus of the present invention in use;
FIG. 3 is a schematic diagram showing the result of the device of the present invention.
The drawing is marked with: 1. the device comprises a heat insulation pipe, 2, a low-temperature bottom plate, 3, a stock solution inlet, 4, a purified solvent outlet, 5, a concentrated product outlet, 6, a pressure regulating valve, 7, a rotor, 8, a mesh grid, 9, nucleating agent crystal particles, 10, scale bars, 11, a matrix solvent, 12, colloidal particles, 13, a concentrated suspension, 14 and a solidification cabin.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
As shown in FIG. 1, the present application proposes a directional solidification segregation apparatus of a colloidal particle system, comprising a heat-insulating pipe 1 and a low-temperature bottom plate 2 arranged at the bottom of the heat-insulating pipe 1, wherein a columnar solidification chamber 14 is formed inside the heat-insulating pipe 1, and a scale bar 10 is arranged on the heat-insulating pipe 1. The solidification compartment 14 is provided with a dope inlet 3, a purified solvent outlet 4, a concentrated product outlet 5, and a pressure adjusting means, which may be a pressure adjusting valve 6. An isolation area is arranged at the bottom of the solidification cabin 14, nucleating agent crystal particles 9 are arranged in the isolation area, the nucleating agent crystal particles 9 and the stock solution are isolated through a mesh grid 8, wherein colloidal particles 12 can pass through the mesh grid 8, and the nucleating agent crystal particles 9 cannot be formed. The solidification chamber 14 is also provided with a rotor 7 rotating in the opposite direction. The device is integrally placed on a temperature control platform and can be in direct contact with the low-temperature bottom plate 2 through heat-conducting glue.
The thermal insulation 1 of the coagulation chamber 14 is a metal tube or a glass tube coated with a porous material layer, or directly a poor thermally conductive polymer tube (e.g. PVC, PTFE, etc.). The low-temperature bottom plate 2 of the solidification cabin 14 is made of heat-conducting metal or semiconductor, has good chemical stability and is not easy to be corroded or oxidized by stock solution.
The solidification cabin 14 is an integrated metal pipe with an open top (a heat insulating material needs to be coated outside the pipe), or the low-temperature bottom plate 2 and the heat insulating pipe 1 are independent parts, and the heat insulating pipe 1 is vertically arranged and connected with the low-temperature bottom plate 2 through a flange gasket structure. The ambient gas in the coagulation chamber 14 may be air, inert to the oxidizing or other reactive components of the dope.
The size of the net grid 8 is smaller than the inner diameter of the solidification cabin 14, and the net grid is fixed at the bottom of the solidification cabin 14 close to the edge in a counterweight, welding or gluing mode. The mesh 8 has a pore size smaller than the size of the nucleating agent crystal particles 9. The nucleator crystals can substantially reduce the critical supercooling degree, so that the solidification nucleation starts at the isolated region and moves along the direction of the solidification compartment 14. The nucleating agent crystal particles 9 can adopt silver iodide and silver bromide crystals with the particle size of 10 nanometers to 1 millimeter according to the variety difference of the matrix solvent 11, such as water-based stock solution, and can also directly use ice crystals as solidification nuclei without limiting the size.
The rotor 7 is a floating electromagnetic rotor or a position-defined mechanical rotor. For different sizes of the coagulation chamber 14, a single rotor 7 or a plurality of rotors 7 can be selected, and the rotating speed is 1 r/min-1000 r/s. If an even number of rotors 7 are provided, they are floated or fixed on the upper portion of the solidification chamber 14, and are symmetrically placed along the radial direction.
A directional solidification segregation method of a colloidal particle system using the above apparatus comprises:
s1, injecting a colloidal particle stock solution (colloidal particle system) into the solidification cabin 14, adjusting the temperature of the low-temperature bottom plate to be lower than the equilibrium state solidification point after the liquid level is stable, establishing a unidirectional temperature gradient in the solidification cabin 14 through the combination of the low-temperature bottom plate 2 and the heat insulation pipe 1, ensuring that the solidification front surface is pushed along the direction, and facilitating the separation of a concentrated product and a purified solvent in the later period;
s2, as shown in figure 2, a vortex flow field is generated in a liquid phase region through the rotor 7 which reversely rotates near a gas-liquid interface to assist the transportation of segregation particles, and the interface fracture or delamination caused by the accumulation of high-concentration particles on a solidification front surface is prevented;
s3, after the stock solution with a certain proportion is solidified, pressurizing and extracting the concentrated suspension liquid 13 through a vacuum pump or the interior of a solidification cabin 14;
s4, the low temperature soleplate 2 is heated to melt the solidified phase, and the purified matrix solvent 11 is extracted, as shown in fig. 3.
During the solidification, melting and extraction, the pressure in the solidification chamber 14 is regulated by means of a pressure regulating valve 6 located at the top.
The matrix solvent 11 of the colloidal particle stock solution is water, a single organic solvent, a mixed organic solvent or liquid metal. The colloidal particles 12 of the colloidal particle stock solution are solid particles, microbubbles, microdroplets, soluble macromolecules or ions.
Example one
The purification and isolation of aqueous cell culture media in biochemical preparation and testing are exemplified.
The colloidal particle stock solution is a cell culture solution, the main components are water (matrix solvent 11), suspended cell communities (colloidal particles 12), and the nucleating agent crystal particles 9 adopt silver iodide crystal particles, and the separation and purification method comprises the following steps:
(1) silver iodide crystal particles are placed in a mesh 8, cell culture fluid is injected along a stock solution inlet 3, and after the liquid level is stable, the temperature of a low-temperature bottom plate 2 is adjusted to be lower than the equilibrium state freezing point TmA temperature gradient along the single direction of the heat insulation pipe 1 is formed in the solidification cabin 14, and the pressure of the solidification cabin 14 is adjusted through the pressure adjusting valve 6 in the process;
(2) the solidification nucleation is triggered on the surface of the nucleating agent crystal, a continuous and stable solidification front is rapidly formed and passes through the grid 8 and is transferred along the temperature gradient, the cell group is separated from the matrix solvent 11 water under the action of solidification segregation, the floating electromagnetic rotor reversely rotates in a liquid phase area to form an eddy current, the segregated cells are rapidly diffused, a accumulation layer is prevented from being formed near the solidification front, and the pressure of the solidification cabin 14 is adjusted by the pressure adjusting valve 6 in the process;
(3) according to the number of the scale bar 10, when the coagulation front is pushed to a preset position, the concentrated cell suspension is extracted through a concentrated product outlet 5;
(4) the low-temperature bottom plate 2 is heated to melt the solidified matrix solvent 11, the purified matrix solvent 11 is extracted through the purified solvent outlet 4, and the pressure of the solidification chamber 14 is adjusted through the pressure adjusting valve 6 in the process.
Example two
The low-temperature crystallization seawater is used as an example.
The colloidal particle stock solution is filtered brine, the main components are water (matrix solvent 11), free sodium ions and chloride ions (colloidal particles 12), the nucleating agent crystal particles 9 adopt silver iodide crystal particles, and the separation and purification method comprises the following steps:
(1) silver iodide crystal particles are placed in a grid 8, brine is injected along a stock solution inlet 3, and after the liquid level is stable, the temperature of a low-temperature bottom plate 2 is adjusted to be lower than the equilibrium state freezing point TmA temperature gradient along the single direction of the heat insulation pipe 1 is formed in the solidification cabin 14, and the pressure of the solidification cabin 14 is adjusted through the pressure adjusting valve 6 in the process;
(2) the solidification nucleation is triggered on the surface of the silver iodide crystal, a continuous and stable solidification front is rapidly formed and passes through the grid 8 and is transferred along the temperature gradient, sodium ions and chloride ions are separated from the matrix solvent 11 under the action of solidification segregation, the floating electromagnetic rotor reversely rotates in a liquid phase region to form an eddy current, the segregated sodium ions and chloride ions are rapidly diffused, a accumulation layer is prevented from being formed near the solidification front by the sodium ions and the chloride ions, and the pressure of the solidification cabin 14 is adjusted by the pressure adjusting valve 6 in the process;
(3) according to the number of the scale bar 10, when the solidification front is pushed to a preset position, extracting the concentrated salt solution through a concentrated product outlet 5;
(4) the low-temperature bottom plate 2 is heated to melt the solidified matrix solvent 11, the purified matrix solvent 11 is extracted through the purified solvent outlet 4, and the pressure of the solidification chamber 14 is adjusted through the pressure adjusting valve 6 in the process.
Claims (8)
1. The directional solidification segregation method of the colloid particle system is characterized in that the used directional solidification segregation device comprises a heat insulation pipe (1) and a low-temperature bottom plate (2) arranged at the bottom of the heat insulation pipe (1), a solidification cabin (14) is formed inside the heat insulation pipe (1), the solidification cabin (14) is provided with a stock solution inlet (3), a purified solvent outlet (4), a concentrated product outlet (5) and a pressure regulating device, and a rotor (7) and a grid (8) internally provided with nucleating agent crystal particles (9) are arranged in the solidification cabin (14);
specifically, the method comprises the following steps:
s1, injecting the colloidal particle stock solution into the solidification cabin (14), and adjusting the temperature of the low-temperature bottom plate (2) to be lower than the solidification point of the equilibrium state after the liquid level is stable;
s2, generating a vortex flow field in a liquid phase region through a rotor (7) which reversely rotates near a gas-liquid interface to assist the transportation of segregation particles;
s3, after the stock solution with a certain proportion is solidified, extracting the concentrated suspension (13);
s4, heating the low-temperature soleplate (2) to melt the solidified phase, and extracting the purified matrix solvent (11);
wherein the colloidal particles (12) can pass through the mesh grid (8), the nucleating agent crystal particles (9) can not pass through the mesh grid (8), and the rotor (7) is provided with an even number, floats or is fixed on the upper part of the solidification cabin (14) and is symmetrically arranged along the radial direction.
2. The method of directional solidification segregation of a colloidal particle system as set forth in claim 1, wherein said rotor (7) is a floating electromagnetic rotor or a position-defined mechanical rotor.
3. The method of directional solidification segregation in a colloidal particle system as set forth in claim 1, wherein the thermal insulation pipe (1) is a metal pipe, a glass pipe coated with a porous material layer, or a polymer pipe.
4. The method for directional solidification segregation of a colloidal particle system as set forth in claim 1, wherein the heat-insulating pipe (1) is provided with a scale bar (10).
5. The method of claim 1, wherein the low temperature soleplate (2) is made of a heat-conducting metal or semiconductor.
6. The method for directional solidification segregation of a colloidal particle system as set forth in claim 1, wherein the grid (8) is smaller than the inner diameter of the solidification chamber (14) and is fixed to the bottom of the solidification chamber (14) near the edge.
7. The method of claim 1, wherein the matrix solvent (11) of the colloidal particle stock solution is water, a single organic solvent, a mixed organic solvent or a liquid metal.
8. The method of claim 1, wherein the colloidal particles (12) of the colloidal particle stock solution are solid particles, microbubbles, microdroplets, soluble macromolecules or ions.
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