CN115265088A - Directional freezing equipment and aerogel preparation method - Google Patents
Directional freezing equipment and aerogel preparation method Download PDFInfo
- Publication number
- CN115265088A CN115265088A CN202210728877.7A CN202210728877A CN115265088A CN 115265088 A CN115265088 A CN 115265088A CN 202210728877 A CN202210728877 A CN 202210728877A CN 115265088 A CN115265088 A CN 115265088A
- Authority
- CN
- China
- Prior art keywords
- cold plate
- freezing
- copper
- cold
- source container
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000007710 freezing Methods 0.000 title claims abstract description 94
- 230000008014 freezing Effects 0.000 title claims abstract description 94
- 239000004964 aerogel Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052802 copper Inorganic materials 0.000 claims abstract description 79
- 239000010949 copper Substances 0.000 claims abstract description 79
- 239000007788 liquid Substances 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 9
- 239000004519 grease Substances 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 9
- 239000011148 porous material Substances 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 15
- 239000004642 Polyimide Substances 0.000 description 8
- 229920001721 polyimide Polymers 0.000 description 8
- 238000004321 preservation Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 238000005057 refrigeration Methods 0.000 description 6
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 235000011089 carbon dioxide Nutrition 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
- F25D31/00—Other cooling or freezing apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention relates to the technical field of aerogel preparation, in particular to directional freezing equipment and an aerogel preparation method. The equipment comprises a cold source container, at least one freezing mould and a cold plate which is detachably arranged at the top end of the cold source container; at least one vertically arranged copper column is fixedly arranged on the lower side of the cold plate; the freezing mould is arranged on the upper side of the cold plate and corresponds to the copper columns one by one; at least one heat-conducting copper fin is arranged between the cold plate and the copper column; one side edge of the heat conduction copper fin is fixed on the lower side of the cold plate, and the other side edge of the heat conduction copper fin is fixed on the copper column. The heat conducting copper fins improve the heat transfer speed. The equipment can enable the temperature field to have temperature gradient along a single direction, ensure that the growth direction of ice crystals is unchanged, enable the aerogel to have the pore size form of ordered arrangement along the direction of the temperature gradient, and is also beneficial to large-scale directional freezing in batches.
Description
Technical Field
The invention relates to the technical field of aerogel preparation, in particular to directional freezing equipment and an aerogel preparation method.
Background
Aerogel is used as a heat insulation material with good performance, and is increasingly applied to various fields at present.
For different types of aerogels, the microscopic nano-pore structure of the aerogel has an important influence on the thermal conductivity of the aerogel, and the thermal conductivity determines the heat preservation and insulation effect of the aerogel.
The directional freezing technology is that a cold source is arranged on one side of liquid to be frozen, so that ice crystals in the liquid grow orderly from one side to the other side, and the nano apertures in the aerogel can be orderly arranged along one direction, so that the aerogel has good heat conductivity.
However, the directional freezing process is very susceptible, and once interference factors occur, the pore size distribution in the aerogel is changed, so that the heat insulation performance is affected. The prior art has the following defects: firstly, dry ice is generally used as a cold source, the bottom surface of a solution is directly contacted with the dry ice, and no heat insulation measure is arranged between the side surface of a container of liquid to be frozen and the upper surface of the dry ice, so that the distribution of a temperature field in the liquid to be frozen is influenced, the temperature field is not an estimated temperature gradient along a single direction, the growth direction of ice crystals in the solution is changed, and the pore diameter form which is orderly arranged along the temperature gradient direction is not beneficial to obtaining; secondly, the heat conducting area is small, the volume of a cold source is limited, the preparation of a large-volume sample is not facilitated, and the large-scale material preparation is difficult.
Disclosure of Invention
The invention aims to provide directional refrigeration equipment and an aerogel preparation method.
The technical scheme for solving the technical problems is as follows:
the invention provides directional refrigeration equipment, which comprises a cold source container, at least one refrigeration mould and a cold plate, wherein the cold plate is detachably arranged at the top end of the cold source container; at least one copper column which is vertically arranged and extends into the cold source container is fixedly arranged on the lower side of the cold plate; the freezing mould is placed on the upper side of the cold plate; at least one heat conduction copper fin is arranged between the cold plate and the copper column; one side edge of the heat conduction copper fin is fixed on the lower side of the cold plate, and the other side edge of the heat conduction copper fin is fixed on the copper column.
The invention has the beneficial effects that the heat conduction copper fin is arranged between the cold plate and the copper column, so that the speed of transferring heat from the refrigerating liquid to the cold plate is effectively improved; meanwhile, the heat conduction copper fins are simple in structure, small in occupied size, low in influence on the total volume of the freezing liquid, and capable of preventing the problem that the freezing liquid is reduced due to the fact that the heat transfer device is added to affect the directional freezing effect.
The invention can be realized by the following further technical scheme:
further, the heat conduction copper fin is a right triangle, and two adjacent right-angle sides are respectively fixed on the lower side of the cold plate and the copper column.
The beneficial effect of adopting above-mentioned further technical scheme lies in, sets up heat conduction copper fin into right triangle, can effectively increase heat conduction area of heat conduction copper fin, further improves directional frozen efficiency.
Furthermore, the number of the heat conduction copper fins is three, and the heat conduction copper fins are uniformly arranged along the circumferential direction of the copper cylinder.
The further technical scheme has the beneficial effects that the heat conduction copper fins are uniformly distributed in the circumferential direction of the copper column, so that the cold plate in the area can be uniformly heated on the horizontal plane; therefore, the liquid to be frozen is uniformly heated in the horizontal direction, and the effect of directional freezing is prevented from being influenced by the temperature gradient in the horizontal direction when the liquid is directionally frozen in the vertical direction.
Further, the freezing mould comprises a mould bottom plate and a mould side wall which is detachably arranged on the mould bottom plate; a cavity capable of containing a solution to be frozen is arranged between the side wall of the mold and the bottom sheet of the mold, and the top end of the cavity is an open end; the mold base sheet is in contact with the upper side of the cold plate; the absolute value of the difference between the thermal diffusivity of the material of the mold bottom sheet and the thermal diffusivity of the solution to be frozen is a, and the absolute value of the difference between the thermal diffusivity of the material of the mold side wall and the thermal diffusivity of the solution to be frozen is b, wherein a is more than b.
The further technical scheme has the advantages that the temperature gradient in the directional freezing process can be ensured to be in the vertical direction; and the isotherm at the solid interface of the solution to be frozen and the sidewall of the mold is horizontal and approximately linear. If the side wall is made of a material having a large difference between the thermal diffusivity and the thermal diffusivity of the solution to be frozen, the temperature line is bent, thereby affecting the directional freezing effect.
Further, heat-conducting silicone grease or heat-conducting oil is coated between the cold plate and the bottom plate of the mold.
The further technical scheme has the beneficial effects that after the heat-conducting silicone grease or the heat-conducting oil is coated, the freezing mould and the cold plate can be in good thermal contact.
The cold plate and the freezing mould are positioned in the heat-preservation shell.
The beneficial effects of adopting above-mentioned further technical scheme lie in, through setting up the lagging casing, can guarantee that directional freezing process does not receive external environment temperature influence, prevent to treat that freezing solution takes place to conduct heat with the environment in the direction beyond the vertical direction to guarantee that directional freezing has good effect.
Furthermore, the lower extreme of lagging casing is open end, the top edge of cold source container is along its radial outside extension to with lagging casing's lower extreme inside wall lock joint.
The adoption of the further technical scheme has the advantages that the edge of the cold plate on the cold source container can be completely accommodated in the heat-insulating shell, so that the heat-insulating effect is further improved; meanwhile, the edge of the cold source container is fastened with the inner side of the heat preservation shell, so that the heat preservation shell is convenient to disassemble.
Furthermore, the cold source container is a cylindrical box body with an open upper end, the cold plate is positioned on the open edge of the cold source container, and a sealing gasket is arranged between the cold plate and the open edge of the cold source container.
The beneficial effect of adopting the further technical scheme is that the cold source liquid can be sealed.
Furthermore, the bottom of the side wall of the cold source container is provided with a cold source liquid inlet and outlet.
Adopt above-mentioned further technical scheme's beneficial effect to lie in, can supply cold source liquid to get into and discharge cold source container.
The invention provides an aerogel preparation method, which comprises a directional freezing step, wherein the directional freezing step is carried out by adopting the directional freezing equipment.
Drawings
FIG. 1 is a cross-sectional view of the directional freezing apparatus of the present invention;
FIG. 2 is a schematic view of the structure of a freezing mold in the directional freezing apparatus of the present invention;
FIG. 3 is an electron micrograph of an ordered array microstructure of the polyimide aerogel of example 1, with a dimension of 500um, in the aerogel preparation method of the present invention;
FIG. 4 is an electron micrograph of an ordered array microstructure of the polyimide aerogel of example 1, with a dimension of 200um, in the aerogel preparation method of the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a cold source container; 11. sealing gaskets; 12. a cold source liquid inlet and outlet;
2. freezing the mold; 21. a mold bottom sheet; 22. a mold sidewall;
3. a cold plate; 31. a copper pillar; 32. a heat conductive copper fin;
4. and (4) a heat-insulating shell.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
As shown in fig. 1, the directional freezing apparatus of the present invention comprises a cold source container 1, at least one freezing mold 2, and a cold plate 3 detachably mounted on the top end of the cold source container 1; at least one copper column 31 which is vertically arranged and extends into the cold source container is fixedly arranged on the lower side of the cold plate 3; the freezing mould 2 is arranged on the upper side of the cold plate 3; at least one heat conduction copper fin 32 is arranged between the cold plate 3 and the copper column 31; one side edge of the heat-conducting copper fin 32 is fixed on the lower side of the cold plate 3, and the other side edge is fixed on the copper column 31; when in use, the cold source container 1 is filled with cold source liquid, and the freezing mould 2 is filled with liquid to be frozen; the copper column 31 and the heat conduction copper fin 32 are immersed in the cold source liquid, so that the heat is conducted to the cold plate 3, the cold plate 3 is kept at a constant temperature, and the temperature and the cooling rate of the cold plate 3 can be adjusted by adjusting the temperature and the cooling rate of the cold source liquid. The liquid to be frozen is poured into the freezing mould 2 and placed on the cold plate 3, and the cold plate 3 conducts heat from bottom to top to the liquid to be frozen in the freezing mould 2, so that an environment with only bottom refrigeration can be realized, and the liquid to be frozen can be directionally frozen in the vertical direction.
According to the directional freezing equipment, the heat conduction copper fins 32 are arranged between the cold plate 3 and the copper columns 31, so that the speed of transferring heat from the freezing liquid to the cold plate 3 is effectively increased; meanwhile, the heat conduction copper fins 32 are simple in structure, small in occupied size, low in influence on the total volume of the freezing liquid, and capable of preventing the problem that the influence on the directional freezing effect is caused by the fact that the freezing liquid is reduced due to the fact that the heat transfer device is added.
By adopting the directional freezing equipment, the cold plate 3 is arranged between the freezing mould 2 and the cold source liquid, so that the direct contact with the cold source liquid is avoided, a temperature field has a temperature gradient along a single direction, the growth direction of ice crystals is ensured to be unchanged, and the obtained aerogel has an aperture form which is orderly arranged along the temperature gradient direction; in addition, under the condition that the freezing mould 2 and the cold plate 3 are isolated from each other, the freezing efficiency is still ensured through the heat conduction copper fins 32, and large-scale batch oriented freezing is facilitated.
In the above embodiment, preferably, the heat conducting copper fins 32 are right-angled triangles, and two adjacent right-angled edges are respectively fixed on the lower side of the cold plate 3 and the copper column 31; the heat conduction copper fins 32 are arranged to be right-angled triangles, so that the heat conduction area of the heat conduction copper fins 32 can be effectively increased, and the directional freezing efficiency is further improved; meanwhile, in practical use, the copper column 31 is generally difficult to completely immerse in the freezing liquid, so that the heat transfer efficiency of the copper column 31 between the liquid level of the freezing liquid and the lower side surface of the cold plate 3 is slightly low, and after the heat-conducting copper fins 32 of the right-angled triangle are installed, the part receives the heat transfer of the heat-conducting copper fins 32 at the same time, so that the utilization rate of the copper column 31 is improved.
The copper pillar 31 of the present invention may be provided with a plurality of heat conductive copper fins 32 as needed. However, if the number of the heat-conducting copper fins 32 is too small, the auxiliary heat transfer function is low, and if the number of the heat-conducting copper fins 32 is too large, the amount of the cold source liquid is significantly reduced.
Therefore, in the above embodiment, preferably, the number of the heat conducting copper fins 32 is three, and the heat conducting copper fins are uniformly arranged along the circumferential direction of the copper pillar 31; by uniformly arranging the heat-conducting copper fins 32 in the circumferential direction of the copper cylinder 31, the cold plate 3 in the area can be uniformly heated on the horizontal plane; therefore, the liquid to be frozen is uniformly heated in the horizontal direction, and the effect of directional freezing is prevented from being influenced by the temperature gradient in the horizontal direction when the liquid is directionally frozen in the vertical direction.
In another embodiment of the present invention, the number of the heat conducting copper fins 32 is three, two of the heat conducting copper fins are right triangles with the same shape, the other is a right trapezoid, the short side of the right trapezoid is located at the lower side, the long side of the right trapezoid is located at the upper side and is fixedly connected with the cold plate 3, the right side of the right trapezoid is fixedly connected with the copper column 31, and the length of the right side of the right trapezoid is greater than that of the right sides of the two right triangles.
It should be noted that the shape of the heat-conducting copper fins 32 is not specific, as long as it is ensured that the heat-conducting copper fins 32 are immersed in the liquid to about half the depth. In the invention, two right-angled triangle shapes with different sizes are designed, the weight reduction requirement of the heat conduction copper fin 32 is considered, and the used copper sheet raw material is saved.
The number of the copper columns 31 can be set according to actual requirements. In one embodiment of the present invention, the number of the copper pillars 31 is one, and the copper pillars 31 are located at the center of the cold plate 3.
In the above embodiment, preferably, the freezing mold 2 is placed on the upper side of the cold plate 3 in a one-to-one correspondence with the copper columns 31; this can further increase the heat transfer rate.
As shown in fig. 2, in the above embodiment, preferably, the freezing mold 2 includes a mold bottom sheet 21 and a mold side wall 22 detachably mounted on the mold bottom sheet 21; a cavity capable of containing a solution to be frozen is arranged between the side wall 22 of the mold and the bottom sheet 21 of the mold, and the top end of the cavity is an open end; the mold bottom sheet 21 is in contact with the upper side of the cold plate 3; the absolute value of the difference between the thermal diffusivity of the material of the bottom mold sheet 21 and the thermal diffusivity of the solution to be frozen is a, the absolute value of the difference between the thermal diffusivity of the material of the side mold wall 22 and the thermal diffusivity of the solution to be frozen is b, and the value of b is close to 0, that is, the thermal diffusivity of the material of the side mold wall 22 is approximately equal to the thermal diffusivity of the solution to be frozen, so a is far greater than b.
In the freezing mould 2, the thermal diffusivity of the mould bottom sheet 21 is far greater than that of the solution to be frozen, and the thermal diffusivity of the mould side wall 22 is similar to that of the solution to be frozen, so that the temperature gradient is in the vertical direction in the directional freezing process; also, the isotherm at the solid interface of the solution to be frozen and the mold sidewall 22 is horizontal and approximately linear. If the mold side wall 22 is made of a material having a thermal diffusivity that is significantly different from the thermal diffusivity of the solution to be frozen, the temperature lines will be bent, thereby affecting the directional freezing effect.
The freezing mould 2 of the invention can select different mould side wall 22 materials according to different thermal diffusivity of the solution to be frozen aiming at the directional freezing process.
In the above embodiment, preferably, the mold side wall 22 and the mold bottom sheet 21 may be connected by sealing and bonding, or may be connected by common mounting methods such as fastening and clamping.
In the above embodiment, preferably, the bottom plate 21 is made of red copper, and the sidewall 22 is made of one of teflon and organic glass.
The cavity in the freezing mold 2 of the present invention may be in various shapes. In one embodiment of the present invention, the freezing mold 2 is cylindrical, and the cylindrical freezing mold 2 can provide a better directional freezing effect for the liquid to be frozen in the vertical direction.
In the above embodiment, it is preferable that the diameter of the freezing mold 2 is 20cm.
The cold plate 3 and the die bottom sheet 21 can be in direct contact with each other, and heat conduction silicone grease or heat conduction oil can be coated on the cold plate; after heat-conducting silicone grease or heat-conducting oil is coated, good thermal contact can be achieved between the freezing mould 2 and the cold plate 3.
The cold source container also comprises a heat insulation shell 4, wherein the heat insulation shell 4 is detachably arranged at the top of the cold source container 1, and the cold plate 3 and the freezing mould 2 are positioned in the heat insulation shell 4; through setting up heat preservation shell 4, can guarantee that directional freezing process does not receive external environment temperature to influence, prevent to treat that freezing solution takes place to conduct heat with the environment in the direction beyond the vertical direction to guarantee that directional freezing has good effect.
In the above embodiment, preferably, the lower end of the thermal insulation casing 4 is an open end, and the top edge of the cold source container 1 extends outwards along the radial direction thereof; the top end edge of the cold source container 1 is fastened with the inner side wall of the lower end of the heat preservation shell 4; the structure can ensure that the edge of the cold plate 3 positioned on the cold source container 1 is completely accommodated in the heat-insulation shell 4, thereby further improving the heat-insulation effect; meanwhile, the edge of the cold source container 1 is fastened with the inner side of the heat preservation shell 4, so that the heat preservation shell 4 is convenient to detach.
In the above embodiment, it is preferable that a sealing gasket 11 is disposed between the cold source container 1 and the cold plate 3, so that the cold source liquid can be sealed.
In the above embodiment, preferably, the bottom of the sidewall of the cold source container 1 is provided with a cold source liquid inlet and outlet 12; the cold source liquid inlet and outlet 12 can supply the cold source liquid to enter and exit the cold source container 1.
In the above embodiment, preferably, the cold source liquid inlet/outlet 12 is communicated with a refrigeration cycle machine, and the refrigeration cycle machine can cool the cold source liquid in the cold source container 1.
In the above embodiment, the material of the cold plate 3 is preferably copper.
According to the preparation method of the aerogel, the prepared aerogel precursor solution is directionally frozen by adopting the directional freezing equipment, so that the aerogel with pore diameter gradient distribution along a single direction is obtained, and the aerogel has good heat conductivity and heat insulation effect.
The working process and effect of the directional freezing apparatus of the present invention will be illustrated by the following examples.
Example 1
In this example, polyimide aerogel was prepared using the directional freezing apparatus of the present invention.
Specifically, the directional freezing equipment of this example directionally freezes a dispersion of polyimide fibers, which contains polyimide nanofibers, benzoxazine, and 1,4-dioxane. Wherein, the 1,4-dioxane has the largest content, and the freezing mould 2 is selected based on the diffusivity.
1,4-dioxane has a thermal diffusivity of about 0.99X 10-7m2The mold side wall 22 of the freezing mold 2 of this example was made of polytetrafluoroethylene, which has a thermal diffusivity of 1.04X 10, and a thermal diffusivity very close to 1,4-dioxane-7m2/s。
And observing the microstructure of the obtained polyimide nanofiber aerogel after directional freezing.
The general directional freezing equipment can cause that the material can not realize the directional freezing of the complete volume, and the equipment of the embodiment can realize the directional freezing of the complete volume of the material and realize the preparation of the anisotropic pore size of the material.
Fig. 3 and 4 are the microscopic structural views of the polyimide aerogel prepared in example 1. It can be seen that the polyimide aerogel prepared by the directional freezing equipment has an orderly arranged micro-pore structure, which shows that the directional freezing effect is good.
In the description of the present invention, it should be noted that the terms "upper", "lower", "vertical", "horizontal", "top", "bottom", "inner", "outer", "radial", "circumferential", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A directional freezing device comprises a cold source container (1) and at least one freezing mould (2), and is characterized by also comprising a cold plate (3) which is detachably arranged at the top end of the cold source container (1);
at least one vertically arranged copper column (31) extending into the cold source container (1) is fixedly arranged on the lower side of the cold plate (3); the freezing mould (2) is arranged on the upper side of the cold plate (3);
at least one heat conduction copper fin (32) is arranged between the cold plate (3) and the copper column (31); and one side edge of the heat conduction copper fin (32) is fixed on the lower side of the cold plate (3), and the other side edge is fixed on the copper column (31).
2. A directional freezing apparatus according to claim 1 wherein the heat conducting copper fins (32) are right triangles with two adjacent sides fixed to the underside of the cold plate (3) and the copper columns (31), respectively.
3. A directional freezing apparatus according to claim 2, wherein the number of the heat-conducting copper fins (32) is three and is uniformly arranged along the circumference of the copper cylinder (31).
4. A directional freezing apparatus according to any one of claims 1 to 3 wherein the freezing mould (2) comprises a mould base sheet (21) and a mould side wall (22) detachably mounted on the mould base sheet (21); a cavity capable of containing a solution to be frozen is arranged between the side wall (22) of the mould and the bottom sheet (21) of the mould, and the top end of the cavity is an open end; the bottom sheet (21) of the mold is in contact with the upper side of the cold plate (3);
the absolute value of the difference between the thermal diffusivity of the material of the mold bottom sheet (21) and the thermal diffusivity of the solution to be frozen is a, and the absolute value of the difference between the thermal diffusivity of the material of the mold side wall (22) and the thermal diffusivity of the solution to be frozen is b, wherein a is more than b.
5. A directional freezing apparatus according to claim 4, wherein the cold plate (3) and the base plate (21) of the mold are coated with heat conducting silicone grease or oil.
6. The directional freezing equipment according to any one of claims 1 to 3, further comprising a thermal insulation shell (4), wherein the thermal insulation shell (4) is detachably mounted on the top of the cold source container (1), and the cold plate (3) and the freezing mold (2) are positioned in the thermal insulation shell (4).
7. The directional freezing equipment according to claim 6, wherein the lower end of the thermal insulation casing (4) is an open end, and the top edge of the cold source container (1) extends outwards along the radial direction and is fastened with the inner side wall of the lower end of the thermal insulation casing (4).
8. A directional freezing apparatus according to any one of claims 1 to 3, wherein the cold source container (1) is a cylindrical box with an open upper end, the cold plate (3) is located at the open edge of the cold source container (1), and a sealing gasket (11) is arranged between the cold plate (3) and the open edge of the cold source container (1).
9. The directional freezing equipment as claimed in any one of claims 1 to 3, wherein the bottom of the sidewall of the cold source container (1) is provided with a cold source liquid inlet/outlet (12).
10. A method for preparing aerogel, comprising a directional freezing step, wherein the directional freezing step is performed by using the directional freezing apparatus as claimed in any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210728877.7A CN115265088B (en) | 2022-06-24 | 2022-06-24 | Directional freezing equipment and aerogel preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210728877.7A CN115265088B (en) | 2022-06-24 | 2022-06-24 | Directional freezing equipment and aerogel preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115265088A true CN115265088A (en) | 2022-11-01 |
| CN115265088B CN115265088B (en) | 2024-05-10 |
Family
ID=83761541
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210728877.7A Active CN115265088B (en) | 2022-06-24 | 2022-06-24 | Directional freezing equipment and aerogel preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115265088B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140158020A1 (en) * | 2011-02-07 | 2014-06-12 | The Trustees Of Dartmouth College | Ice-Tempered Hybrid Materials |
| CN108767217A (en) * | 2018-05-15 | 2018-11-06 | 武汉科技大学 | A kind of orienting stephanoporate LiFePO4-graphene composite material and preparation method thereof |
| CN109666263A (en) * | 2019-01-04 | 2019-04-23 | 浙江大学 | The preparation method and product of a kind of boron nitride/epoxy resin composite material and application |
| CN111171384A (en) * | 2020-02-10 | 2020-05-19 | 东华大学 | Light warm-keeping flexible chitosan/nano-cellulose aerogel and preparation method thereof |
| CN111795532A (en) * | 2019-04-08 | 2020-10-20 | Ii-Vi特拉华有限公司 | Frozen substance maker |
-
2022
- 2022-06-24 CN CN202210728877.7A patent/CN115265088B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140158020A1 (en) * | 2011-02-07 | 2014-06-12 | The Trustees Of Dartmouth College | Ice-Tempered Hybrid Materials |
| CN108767217A (en) * | 2018-05-15 | 2018-11-06 | 武汉科技大学 | A kind of orienting stephanoporate LiFePO4-graphene composite material and preparation method thereof |
| CN109666263A (en) * | 2019-01-04 | 2019-04-23 | 浙江大学 | The preparation method and product of a kind of boron nitride/epoxy resin composite material and application |
| CN111795532A (en) * | 2019-04-08 | 2020-10-20 | Ii-Vi特拉华有限公司 | Frozen substance maker |
| CN111171384A (en) * | 2020-02-10 | 2020-05-19 | 东华大学 | Light warm-keeping flexible chitosan/nano-cellulose aerogel and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115265088B (en) | 2024-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3569961A1 (en) | Preparation method for loop heat pipe evaporator | |
| CN113089090A (en) | Reaction system | |
| CN115265088A (en) | Directional freezing equipment and aerogel preparation method | |
| CN113308227A (en) | Preparation method and application of high-thermal-conductivity foam composite phase-change material | |
| CN211170961U (en) | Rotating device | |
| CN115124352A (en) | Aerogel with double-orientation network and preparation method and application thereof | |
| CN216778769U (en) | Heat transfer rate controllable device for performing bidirectional freezing casting on solution | |
| CN219059209U (en) | Silicon carbide growing device | |
| CN110983403A (en) | Aluminum alloy electrolytic oxidation film forming device | |
| CN217210079U (en) | Ultrasonic-assisted freeze drying equipment | |
| CN212057865U (en) | Directional freezing device of thick liquids | |
| CN214668157U (en) | High-low temperature test bed suitable for deformation test of phase change energy storage device | |
| CN215506572U (en) | Constant temperature assembling device for magnetic stirrer | |
| CN113893989A (en) | Novel vacuum humidification coating film making machine | |
| CN113026097A (en) | Rotating device | |
| CN117739589B (en) | Multi-cavity dewar tank based on fixed cold source and temperature regulating system | |
| CN210718073U (en) | Gas quick heating device | |
| CN107507948A (en) | Phase change device and power battery module | |
| CN207133674U (en) | It is a kind of can Quick temperature adjustment lifting electric hot water bath | |
| CN217068828U (en) | High-flux reaction kettle | |
| CN213119714U (en) | Directional freezing device for preparing inorganic powder crystal grains | |
| CN211936819U (en) | Heat exchange system for ultrahigh pressure refrigeration equipment and ultrahigh pressure refrigeration equipment | |
| CN212141540U (en) | Self-circulation secondary heat exchange gradient crystallization device | |
| CN214765388U (en) | Chemical reaction kettle for downhole operation | |
| CN219116250U (en) | Chocolate storage insulation bin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |