CN111690378A - Ultralow-temperature micro-nano fluid and preparation method thereof - Google Patents
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Abstract
The invention discloses an ultralow temperature micro-nano fluid which is a mixture of a solid first material and a liquid second material; wherein the first material has a melting point greater than-130 ℃; the melting point of the second material is lower than-130 ℃; in the ultralow temperature micro-nano fluid, the density ratio of the first material to the second material is 1 (0.8-1.1). The invention also provides a preparation method of the ultralow-temperature micro-nano fluid. The ultralow-temperature micro-nano fluid can be used for freezing biological materials, does not leave any pollution source after evaporation, and has good component stability and no obvious Layton phenomenon.
Description
Technical Field
The invention belongs to the field of preparation of ultralow-temperature materials, and particularly relates to an ultralow-temperature micro-nano fluid and a preparation method thereof.
Background
The heat transfer efficiency of the two-phase fluid formed by adding particles into the liquid is improved, and the nano fluid and the solid-liquid binary ice slurry which are firstly proposed by Choi et al in Argonne national laboratories in America have been widely researched as refrigerants from Maxwell (1873) to 90 th 20 th century so as to improve the heat transfer and heat storage efficiency. Generally, micro-nano fluid disperses metal or nonmetal powder into traditional heat exchange media such as water, alcohol, oil and the like to prepare a novel uniform, stable and high-heat-conductivity heat exchange medium, and the applications are limited to the conditions above normal temperature.
The preparation method of the micro-nano fluid mainly comprises two steps: one-step and two-step processes. The one-step method is to complete the preparation process of the micro-nano particles and the dispersion process of the micro-nano particles in the base liquid at the same time. The two-step method disperses the prepared micro-nano particles into the base liquid by a certain means, and the preparation and dispersion processes are carried out in two steps. The one-step preparation process is complex, the required equipment is expensive, and the capacity of mass production is not available, so that the nanofluid is mainly prepared by a two-step method at the present stage. Nanoparticles in the nanofluid prepared by the two-step method are easy to self-polymerize, and the polymerized micro-nanoparticles can be separated out from the base liquid after being placed for a long time.
In general, the heat transfer coefficient of ultra-low temperature fluids (especially liquid simple substances) is very low, for example, the heat transfer coefficient of liquid nitrogen is 0.145W/m.K, and the heat transfer coefficient of liquid argon is 0.129W/m.K. The heat transfer coefficient of the solid is high, for example, the heat transfer coefficient of the solid ice is 2.25-3.5W/m.K.
When the refrigerant is used as a refrigerant, the solid shape is fixed, the refrigerant is not easy to be tightly attached to a container, and the liquid refrigerant has the fluid characteristic and has application scenes which are not possessed by the solid refrigerant. However, the liquid refrigerant has a low heat transfer coefficient, and if the contact surface between the liquid refrigerant and the object to be processed is subjected to the leyton phenomenon, the heat transfer effect of the liquid refrigerant is further reduced.
Even if the stability and the dispersibility of the micro-nano fluid formed by the solid particles and the liquid are difficult to guarantee at normal temperature, the stability and the dispersibility of the micro-nano fluid are difficult to guarantee at low temperature of-150 ℃ and-130 ℃, and the heat transfer coefficient of the liquid cannot be uniformly reduced by the solid floating on the liquid surface or separated out from the bottom layer of the liquid.
In the prior art, no report that micro-nano fluid which is mixed with solid and liquid at the temperature of-130 ℃ or lower and exists stably is taken as a refrigerant is found.
Disclosure of Invention
In order to solve the problems of stability and dispersibility of the existing micro-nano fluid, the invention provides an ultralow temperature micro-nano fluid in a first aspect, wherein the ultralow temperature micro-nano fluid is a mixture of a solid first material and a liquid second material, and the solid first material is suspended in the liquid second material in micron-sized and/or nano-sized solid particles;
wherein the first material has a melting point higher than-130 ℃ (e.g., -30 ℃, -40 ℃, -50 ℃, -60 ℃, -70 ℃, -80 ℃, -90 ℃, -100 ℃, -110 ℃, -120 ℃, -130 ℃);
the melting point of the second material is lower than-130 ℃ (e.g., -130 ℃, -140 ℃, -160 ℃, -170 ℃, -180 ℃, -190 ℃, -200 ℃, -210 ℃); and is
In the ultralow-temperature micro-nano fluid, the density ratio of the first material to the second material is 1 (0.8-1.1).
The purpose of preparing the ultralow-temperature stable micro-nano fluid is achieved by selecting the first material and the second material with similar densities.
In some embodiments, the second material comprises a group a material and a group B material: the group a material is a material or mixture of materials having a density greater than the first material in a solid state at a temperature at which the second material is in a liquid state; the group B material is a material or mixture of materials having a density less than the first material in a solid state at a temperature at which the second material is in a liquid state.
In some embodiments, the melting point of the first material is the melting point at normal atmospheric pressure; and/or the melting point of the second material is the melting point at normal atmospheric pressure.
In some embodiments, the density ratio of the first material in the solid state to the second material in the liquid state is 1:0.90, 1:0.91, 1:0.92, 1:0.93, 1:0.94, 1:0.95, 1:0.96, 1:0.97, 1:0.98, 1:0.99, or 1: 1.
In some embodiments, the boiling point of the first material is equal to or less than 110 ℃ and/or the boiling point of the second material is equal to or less than 0 ℃.
In some embodiments, the boiling point of the first material is the boiling point at normal atmospheric pressure; and/or
The boiling point of the second material is the boiling point at normal atmospheric pressure.
In some embodiments, the first material is ice and the group B material of the second material is a mixture of ethane and one or both of nitrogen; the group A material of the second material is one or a mixture of two of argon and krypton.
In some embodiments, the first material is ice and the second material is a mixture of nitrogen and argon.
In some embodiments, the volume ratio of the nitrogen to the argon in the liquid state is (4-6):1, preferably 5: 1.
In some embodiments, the first material is ice and the second material is a mixture of ethane and argon.
In some embodiments, the volume ratio of ethane to argon in the liquid state is 5 (3-5), more preferably 5: 4.
In some embodiments, the first material is carbon dioxide and the group B material of the second material is one, two or three of argon, nitrogen and ethane; the group A material is krypton.
In some embodiments, the first material is carbon dioxide and the second material is a mixture of argon and krypton.
In some embodiments, the liquid-state volume ratio of argon to krypton is (9-12) to 1, preferably 10 to 1.
In some embodiments, the volume ratio of the first material in the solid state to the second material in the liquid state is 1 (20-100), preferably 1:50, to achieve a stable desired nanofluid, which can ensure both fluidity and heat transfer effect.
The second aspect of the present invention provides a preparation method of the ultralow temperature micro-nano fluid according to the first aspect of the present invention, the preparation method comprising the following steps:
introducing nitrogen, helium or argon into the first material in a liquid state, and collecting a gaseous mixture A;
introducing the mixture A into a liquid second material to obtain the ultralow-temperature micro-nano fluid;
alternatively, the preparation method comprises the following steps:
mixing the first material with the second material to obtain a mixture B;
and reducing the temperature of the mixture B to a temperature at which the second material is in a liquid state and the first material is in a solid state, so as to obtain the ultralow-temperature micro-nano fluid.
The third aspect of the present invention provides the use of the ultra-low temperature micro-nano fluid of the first aspect of the present invention in the following aspects:
freezing the biological material;
preserving the food;
and (5) cutting the metal at low temperature.
The ultralow-temperature micro-nano fluid can be used for preparing a cryoelectron microscope (cryoEM) sample of biological medicines, viruses and biomacromolecules and quickly freezing germ cells.
Compared with the prior art, the invention has the following beneficial effects:
1. the cold source micro-nano material has the advantages that the difference between the solid phase formed by the first material and the liquid phase density phase formed by the second material is not large, the materials can be uniformly mixed, layering is avoided, and the storage is stable.
2. The cold source nanometer material of the invention adopts carbon dioxide or ice to form micron or nanometer particles, so the nanometer material can be evaporated along with the cold source without leaving any pollutant, can avoid the defect of adopting silicon dioxide nanometer particles, and is very suitable for the application in the field of biological medicine.
3. The invention adopts proper steps and parameters in the preparation process, and the synergistic effect is realized, so that the production efficiency of the cold source material is improved.
4. The method is simple and easy to implement, low in cost, convenient for industrial production and suitable for popularization and use.
5. The solid particles in the fluid of the ultra-low temperature cold source are uniformly dispersed in the liquid, so that the heat transfer coefficient of the liquid is obviously increased, the temperature of the fluid of the ultra-low temperature cold source is uniformly and quickly reduced, and the Ladun phenomenon generated by the fluid of the pure liquid cold source can be weakened or eliminated by the solid particles.
Drawings
Fig. 1 is an appearance picture of a micro-nano fluid according to a first embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Definition of
Ultra-low temperature micro-nano fluid: the ultralow-temperature micro-nano fluid is a solid-liquid mixed fluid under an ultralow temperature condition (such as below 130 ℃), a solid first material is suspended in a liquid second material in the form of micron-sized and/or nanometer-sized solid particles (preferably, the particle size is not higher than 1000 microns), and the cooling temperature of the ultralow-temperature micro-nano fluid provided by the invention can reach the temperature of the liquid second material.
The main principle on which the invention is based
The Stokes settling velocity formula (Stokes formula) is a formula (formula 1) for theoretically calculating the settling velocity (w) of a sphere in a laminar state by the american physicist Stokes (G · Stokes) in 1850.
The formula is as follows: w ═ 2(ρ)S－ρ)gr2]/9μ。
In the formula: rhoSIs the particle density; ρ is the density of water; mu is the fluid viscosity; r is the particle radius; g is the acceleration of gravity. The formula is obtained under the ideal laboratory conditions of still water, constant temperature of 20 ℃, unchanged viscosity of the medium, spherical particles, same density, smooth surface and non-collision of the particles.
In addition, according to Stokes' Law, the precipitation velocity v of particles in a liquid is (formula 2):
wherein, D: the diameter of the particles; ρ: density of solid particles; rhofLiquid density, g gravity acceleration, η liquid viscosity.
Therefore, at ultralow temperature, the solid particles and the liquid are mixed to form ultralow temperature coldThe source fluid can play a role of a cold source, and becomes gas at normal temperature to be volatilized, so that no trace or residue is left. Further, ρ - ρfThe smaller the value of (A), the smaller the settling velocity of the solid particles in the liquid, and when the value is 0, the solid particles and the liquid form a homogeneous fluid, cannot be layered and exist stably.
In addition, the solid particles in the fluid of the ultra-low temperature cold source are uniformly dispersed in the liquid, so that the heat transfer coefficient of the liquid is remarkably increased, the temperature of the fluid of the ultra-low temperature cold source is uniformly and quickly reduced, and the phenomenon of Laden caused by the fluid of the pure liquid cold source can be weakened or eliminated by the solid particles.
Example one
The first material of this embodiment is water, and the second material is nitrogen and argon, wherein the nitrogen and argon are taken according to the dosage that the volume ratio of liquid nitrogen to liquid argon is 5:1, and the water is taken according to the volume ratio of solid ice to the mixed liquid composed of liquid nitrogen and liquid argon is 1: 50.
(1) Mixing: and mixing liquid nitrogen and liquid argon in a vacuum heat-insulating container according to a volume ratio at the temperature of-196 ℃ to obtain the mixed cryogenic fluid.
(2) And (3) solidification: introducing nitrogen into liquid water at normal temperature to obtain nitrogen containing saturated moisture, and introducing the nitrogen containing saturated moisture into mixed low-temperature fluid to obtain ice micro-nano fluid, also called mixed micro-nano particle slurry, which is a uniform mixture.
At this time, the mixture becomes a mixed fluid containing fine ice particles, liquid nitrogen, and liquid argon.
The density of solid ice particles in formula 2 is rho 0.9g/cm3Mixed liquid of liquid nitrogen and liquid argon ρfThe density is about 0.9g/cm3。
Therefore V ≈ 0, the ice particles in the fluid mixture will not settle and can be stably present, and a photograph of the fluid is shown in fig. 1.
Example two
The first material of this embodiment is water, and the second material is ethane and argon, wherein the ethane and argon are taken out according to the usage amount of liquid ethane and liquid argon in the volume ratio of 5:4, and the water is taken out according to the volume ratio of solid ice and the mixed liquid composed of liquid ethane and liquid argon of 1: 50.
(1) Mixing: the ethane gas and the argon gas were made into a mixture of ethane gas and argon gas.
(2) Low-temperature liquefaction: and (2) adopting liquid nitrogen with the temperature of minus 196 ℃ as a refrigerant, contacting the mixture with the inner wall surface of a container with the temperature of minus 196 ℃, and reducing the gas temperature to minus 186 ℃ to obtain the liquid ethane-liquid-argon mixed fluid.
(3) And (3) solidification: introducing nitrogen gas into liquid water at normal temperature to obtain nitrogen gas containing saturated moisture, and introducing the nitrogen gas containing saturated moisture into liquid ethane-liquid-argon mixed fluid to obtain ice micro-nano fluid, also called mixed micro-nano particle liquid slurry, which is a uniform mixture.
At this time, the mixture becomes a mixed fluid containing fine ice particles, liquid ethane, and liquid argon.
The density of solid ice particles in formula 2 is rho 0.9g/cm3Liquid ethane and liquid argon mixture ρfThe density is about 0.9g/cm3。
Therefore, V ≈ 0, ice particles in the fluid mixture will not settle and can exist stably.
EXAMPLE III
In this embodiment, the first material is carbon dioxide, and the second material is argon and krypton, wherein the argon and krypton are taken according to the usage amount of the liquid argon to the liquid krypton in the volume ratio of 10:1, and the carbon dioxide is taken according to the volume ratio of the solid carbon dioxide to the mixed liquid composed of the liquid argon and the liquid krypton of 1: 50.
(1) Gas mixing: and preparing the carbon dioxide gas, the argon gas and the krypton gas into a mixed gas of the carbon dioxide gas, the argon gas and the krypton gas.
(2) Low-temperature liquefaction: and (2) adopting liquid nitrogen with the temperature of minus 196 ℃ as a refrigerant, contacting the mixed gas with the inner wall surface of the container with the temperature of minus 196 ℃, and reducing the temperature to minus 186 ℃ to obtain carbon dioxide micro-nano fluid, namely mixed micro-nano particle slurry, which is uniform mixed liquid.
At this time, the mixed gas becomes a mixed gas stream containing carbon dioxide fine particles, argon gas, and krypton gas.
The density of the solid carbon dioxide particles in the formula 2 is rho-1.56 g/cm3Mixed liquid of liquid ethane and liquid krypton ρfThe density is about 1.56g/cm3。
Therefore, V ≈ 0, the carbon dioxide particles in the fluid mixture will not settle and can exist stably.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (10)
1. The ultralow-temperature micro-nano fluid is a mixture of a solid first material and a liquid second material, wherein the solid first material is suspended in the liquid second material in micron-scale and/or nanometer-scale solid particles;
wherein the first material has a melting point greater than-130 ℃;
the melting point of the second material is lower than-130 ℃; and is
In the ultralow-temperature micro-nano fluid, the density ratio of the first material to the second material is 1 (0.8-1.1).
2. The ultra-low temperature micro-nano fluid of claim 1, wherein:
the second material comprises a group A material and a group B material: the group a material is a material or mixture of materials having a density greater than the first material in a solid state at a temperature at which the second material is in a liquid state; the group B material is a material or mixture of materials having a density less than the first material in a solid state at a temperature at which the second material is in a liquid state.
3. The ultra-low temperature micro-nano fluid of claim 1 or 2, wherein:
the melting point of the first material is the melting point at normal atmospheric pressure; and/or
The melting point of the second material is the melting point at normal atmospheric pressure.
4. The ultra-low temperature micro-nano fluid of claim 1 or 2, wherein:
the density ratio of the first material in the solid state to the second material in the liquid state is 1:0.90, 1:0.91, 1:0.92, 1:0.93, 1:0.94, 1:0.95, 1:0.96, 1:0.97, 1:0.98, 1:0.99, or 1: 1.
5. The ultra-low temperature micro-nano fluid of claim 1 or 2, wherein:
the boiling point of the first material is equal to or lower than 110 ℃, and/or
The second material has a boiling point equal to or lower than 0 ℃.
6. The ultra-low temperature micro-nano fluid of claim 5, wherein:
the boiling point of the first material is the boiling point at normal atmospheric pressure; and/or
The boiling point of the second material is the boiling point at normal atmospheric pressure.
7. The ultra-low temperature micro-nano fluid of claim 2, wherein:
the first material is ice and the group B material of the second material is a mixture of one or two of ethane and nitrogen; the group A material of the second material is one or a mixture of two of argon and krypton;
preferably, the first material is ice and the second material is a mixture of nitrogen and argon; preferably, the volume ratio of said nitrogen to said argon in the liquid state is (4-6: 1, more preferably 5: 1;
preferably, the first material is ice and the second material is a mixture of ethane and argon; preferably, the volume ratio of ethane to argon in the liquid state is 5 (3-5), more preferably 5: 4;
preferably, the first material is carbon dioxide and the group B material of the second material is one, two or three of argon, nitrogen and ethane; the group A material is krypton;
more preferably, the first material is carbon dioxide and the second material is a mixture of argon and krypton; preferably, the volume ratio of the argon to the krypton in the liquid state is (9-12):1, more preferably 10: 1.
8. The ultra-low temperature micro-nano fluid of claim 1 or 2, wherein:
the volume ratio of the first material in the solid state to the second material in the liquid state is 1 (20-100), preferably 1: 50.
9. The preparation method of the ultralow temperature micro-nano fluid according to any one of claims 1 to 8, comprising the following steps:
introducing nitrogen, helium or argon into the first material in a liquid state, and collecting a gaseous mixture A;
introducing the mixture A into a liquid second material to obtain the ultralow-temperature micro-nano fluid;
alternatively, the preparation method comprises the following steps:
mixing the first material with the second material to obtain a mixture B;
and reducing the temperature of the mixture B to a temperature at which the second material is in a liquid state and the first material is in a solid state, so as to obtain the ultralow-temperature micro-nano fluid.
10. Use of the ultra-low temperature micro-nano fluid according to any one of claims 1 to 8 in the following aspects:
freezing the biological material;
preserving the food;
and (5) cutting the metal at low temperature.
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