CN107033851B - Method for treating surface of phase change composite particle - Google Patents
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Abstract
A method for treating the surface of phase change composite particles comprises the steps of taking a coarse phase change composite component with the granularity of 40-100 meshes from an expanded graphite/paraffin phase change composite, adding a fine phase change composite component with the granularity of 300-800 meshes into an ethanol solution of a binder, and uniformly mixing to obtain a liquid mixture; placing the coarse components of the step 40-100 meshes in a multifunctional coating dryer to enable the coarse components to be in a fluidized state, spraying a liquid mixture onto the surfaces of fluidized particles, drying the materials while spraying, dissolving insulating resin in ethanol, spraying the surfaces of the particles shaped in the fluidized state, drying the materials while spraying, and finally obtaining the product. The invention has the advantages of good stability, high heat conductivity coefficient, good sphericity and surface insulation.
Description
Technical Field
The invention belongs to the technical field of phase-change materials, and particularly relates to a method for treating the surface of phase-change composite particles.
Background
Phase change materials achieve the goal of temperature control by releasing or absorbing heat during the phase transition (solid-liquid). The phase-change technology does not need extra energy and has higher temperature control precision, so the phase-change technology is favored in more and more fields. The commonly used phase-change materials comprise organic phase-change materials and inorganic hydrated salt phase-change materials, the inorganic hydrated salt phase-change materials have high supercooling degree and strong corrosion to metal materials, and the organic phase-change materials represented by paraffin have proper phase-change temperature and low supercooling degree, so the organic phase-change materials gradually become preferred materials in the field of phase-change materials. In order to ensure the integrity of the shape or structure of the material, the phase-change material needs to be compounded with the framework material, so that the phase-change substance is prevented from leaking in the phase-change process. The current common method is to prepare the paraffin into phase-change microcapsules or adopt expanded graphite to adsorb the paraffin, so as to solve the problem of leakage of the phase-change material in the process of energy storage and energy release. Chinese patent CN106433567A reduces the inelastic deformation of paraffin wax caused by volume change in the phase change process by coating two layers of resin on the surface of emulsion paraffin wax. Chinese patent CN1294229C compressed the expanded graphite by piston extrusion to obtain compressed expanded graphite, and absorbed paraffin in the expanded graphite by common or vacuum infiltration, which solves the problem of paraffin leakage in the phase change process to a greater extent.
One of the problems that must be solved in the application and popularization of phase change materials is the heat transfer performance and stability (leakage) of the materials. At present, the core body of the microcapsule material is paraffin with very low heat conductivity, and the shell is also a resin material with poor heat conductivity. The phase-change composite material prepared by the method has relatively common heat-conducting property, and meanwhile, the microcapsule is of a core-shell structure, the inside of the microcapsule is completely composed of paraffin, and large stress is generated due to volume change in the phase-change process, so that the shell is cracked or damaged. The expanded graphite/paraffin phase-change material has good heat conduction and stability, and needs to be crushed and compounded in some application occasions, but the crushed particles have complex shapes and poor sphericity, are not beneficial to outer-layer coating insulation and closest packing compounding, and limit the application of the expanded graphite/paraffin phase-change material in some occasions needing heat conduction and insulation.
Disclosure of Invention
The invention aims to provide a method for treating the surface of phase-change composite particles with good stability, high heat conductivity coefficient, good sphericity and surface insulation.
In order to achieve the above object, the present invention provides a method comprising the steps of:
(1) crushing and screening the expanded graphite/paraffin phase-change composite material, and taking 100 parts by mass of a coarse component of the phase-change composite material with the granularity range of 40-100 meshes and 15-40 parts by mass of a fine component of the phase-change composite material with the granularity range of 300-800 meshes;
(2) dissolving 10-30 parts by mass of a binder in 2-5% of ethanol, weighing the 800-mesh fine component obtained in the step (1), slowly adding an ethanol solution of the binder, and uniformly mixing to obtain a liquid mixture;
(3) placing the coarse components of the phase-change composite material with the size of 40-100 meshes obtained in the step (1) in a multifunctional coating dryer to enable the coarse components to be in a fluidized state, spraying the liquid mixture obtained in the step (2) onto the surfaces of fluidized particles, and drying the material while spraying;
(4) and (3) fully dissolving 5-8 parts of insulating resin in 2-5% of ethanol by mass, spraying the insulating resin on the surface of the shaped particles in the fluidized state in the step (3), and drying the material while spraying to obtain the product.
The expanded graphite/paraffin phase-change composite material is obtained by adopting a Chinese patent CN1294229C infiltration method.
The binder is thermosetting epoxy resin or phenolic resin;
the conditions for the spraying in the step (3) as described above are: the spraying speed of the liquid mixture is 150-350 ml/h; setting the air inlet temperature to be 5-15 ℃ higher than the phase change temperature, and drying for 1-4h to obtain the shaped phase change composite particles.
The spraying conditions of the step (4) as described above are: the spraying speed of the insulating resin ethanol solution is 100-250ml, the drying temperature of the spraying is 5-15 ℃ higher than the phase transition temperature, and the drying time is 1-2h, so that the final product is obtained.
The common coating adopts the adhesive such as acrylic resin, hydroxymethyl cellulose and the like, has poor heat resistance and belongs to thermoplastic resin, and the adopted phase-change material has large volume change before and after phase change, so the thermoplastic resin can deform and even be burst at high temperature, and the resin can not play a role in stability. Therefore, the invention adopts thermosetting resin epoxy resin or phenolic resin, and the invention can keep a hard shape even at higher use temperature, thereby improving the stability of the product.
The coarse particles adopted by the invention are 40-100 meshes, and the fine particles are 300-800 meshes. Because the phase change particles are obtained by mechanical crushing, the surface appearance is poor, and the shape profile is high. Therefore, if the diameter of the fine particles is too large, the particle size of the shaped particles is inevitably large, and the gaps between the particles are large, so that the diameter of the fine particles used is smaller than 300 mesh. The micropore structure of the expanded graphite is generally about 10-15 μm, so that the phase-change material is adsorbed, and when the particle diameter is near the micropore diameter, the micropore is easy to break, so that the adsorption capacity is reduced, and therefore, the diameter of the fine particle is larger than 800 meshes.
The concentration of the adopted adhesive and insulating resin dissolved in ethanol is 2-5 wt%, and when the concentration is less than 2 wt%, the coating speed is too slow, and the efficiency is lower. The treatment idea of the invention is that the solution is sprayed on the coarse particles in the fluidization state process, and the binder is solidified while the solvent is removed; when the concentration is more than 5 wt%, blocking easily occurs between the particles having the surface coated with the binder in the case of collision in a fluidized state.
The spraying speed in the step (3) is 150-350ml/h, and when the spraying speed is less than 150ml/h, the treatment capacity is low, and the efficiency is low; when the spraying speed is more than 350ml/h, the solution of fine particles on the surfaces of the coarse particles is more, the curing time of the resin is prolonged, and the coarse particles collide in the fluidization process to cause the adhesion phenomenon.
The spraying speed in the step (4) of the invention is 100-250ml/h, compared with the step (3), the specific surface area of the particles is smaller than that in the step (3), so that the spraying speed needs to be reduced, the spraying speed is too high, the resin is not cured completely, and the particles collide in the fluidization process to cause adhesion.
The air inlet temperature in the spraying process of the steps (3) and (4) of the invention is selected within the range of 5-15 ℃ higher than the phase change temperature. When the temperature difference between the inlet air temperature and the phase change temperature is less than 5 ℃, the treatment efficiency is reduced, and the resin can be cured to cause adhesion. When the difference between the inlet air temperature and the phase change temperature is larger than 15 ℃, although the contact time of hot air and particles is short, the surface temperature of the particles is probably lower than the set temperature, the excessively high inlet air temperature can make the surface temperature of the phase change material particles larger than the phase change temperature, so that the phase change occurs and the leakage is caused.
The binder and the insulating resin material adopted in the steps (3) and (4) are the same resin, and the same resin has good compatibility, so that the integrity of the material is kept, and the core-shell phase separation cannot occur after multiple thermal cycles.
Compared with the prior art, the invention has the following advantages:
1. compared with the microcapsule without surface shaping or a paraffin system, the expanded graphite/paraffin phase change particles obtained by surface treatment by the method have better stability, the leakage rate of the common phase change composite material is 8-15%, and the leakage rate of the phase change composite material obtained by the method can reach 0.89%; the heat conductivity coefficient of the general phase-change microcapsule is less than 0.4W/mK, the heat conductivity coefficient of the expanded graphite phase-change composite material particles subjected to surface shaping is 12-15W/mK, and the heat conductivity coefficient of the expanded graphite phase-change composite material particles subjected to surface treatment is 8-11W/mK. The heat conductivity coefficient of the phase-change composite particles after surface treatment is much higher than that of a paraffin microcapsule system, and the heat conductivity loss is less than that before treatment.
2. Compared with the common expanded graphite/paraffin phase-change composite particles, the phase-change composite material obtained by the prior art has the advantages that the sphericity can be improved to 0.75 or even higher from 0.51 on the premise of small-range loss of heat conductivity, and the higher sphericity is more favorable for outer layer insulation and closest packing and compounding in the subsequent heat-conducting product forming process.
3. The expanded graphite/paraffin phase-change composite particles without surface treatment have good conductivity, and the application range of the expanded graphite/paraffin phase-change composite particles in the electronic field is limited. The phase-change composite particles subjected to surface shaping treatment and secondary surface insulation treatment can achieve complete insulation performance, and can be applied to the field with higher requirements on heat conduction and insulation.
Drawings
FIG. 1 is a schematic view of the intermediate product particles obtained in step (3) of the present invention;
FIG. 2 is a diagram showing the morphology of the expanded graphite/paraffin phase-change composite material after being crushed (a) and the product of the invention (b).
Detailed Description
The invention will be further explained in detail with reference to the drawings and the embodiments without limiting the invention in any way
Example 1
(1) The expanded graphite/paraffin phase-change composite material is obtained by adopting a Chinese patent CN1294229C infiltration method: 30g of flake graphite with the fineness of 50 meshes and the carbon content of 94 percent, 300g of sulfuric acid with the concentration of 98 percent and 20g of potassium permanganate are taken and evenly stirred. Stirring at 45 deg.C and 300RPM for 30min, washing with water, filtering until the final solution has a pH of 4, and oven drying at 60 deg.C for 10 h. Taking 5g of the intercalation in a microwave oven, and carrying out microwave for 30s at 200W to obtain the expanded graphite. The expanded graphite was pressed into an expanded graphite preform at an extrusion rate of 0.2 which is an expansion rate. And (3) at the temperature of 45 ℃, immersing the compressed expanded graphite into molten paraffin with the phase transition temperature of 39 ℃, vacuumizing for 40min under the vacuum pressure of 82KPa, and immersing for 1.5h to obtain the phase transition composite material.
(2) Crushing the phase-change composite material, and then screening, wherein 100 parts by mass of coarse components with the granularity range of 40-60 meshes and 18 parts by mass of fine components with the granularity range of 300-500 meshes are taken;
(3) taking 10 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) as a binder, uniformly mixing, and dissolving in ethanol according to the mass fraction of 3 wt%; taking 18 parts of fine components obtained by screening in the step (2), slowly adding an ethanol solution of a binder, and uniformly mixing to obtain a liquid mixture;
(4) placing 100 parts of the coarse component obtained by screening in the step (2) in a coating dryer to be in a fluidized state, and spraying the liquid mixture obtained in the step (3) onto the surface of particles of the coarse component in the fluidized state at a speed of 200 ml/h; setting the air inlet temperature at 45 ℃, and drying for 2 hours to obtain the shaped phase-change composite material.
(5) And (3) fully dissolving 5 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) in 5% of ethanol, spraying the two-component epoxy resin on the surface of the fluidized and shaped particles in the step (3) at a spraying speed of 125ml/h, setting the air inlet temperature to be 45 ℃, drying the materials while spraying, and drying for 1h to obtain the final product.
Example 2
(1) The expanded graphite/paraffin phase-change composite material is obtained by adopting a Chinese patent CN1294229C infiltration method: 30g of flake graphite with the fineness of 50 meshes and the carbon content of 94 percent, 300g of sulfuric acid with the concentration of 98 percent and 20g of potassium permanganate are taken and evenly stirred. Stirring at 45 deg.C and 300RPM for 30min, washing with water, filtering until the final solution has a pH of 4, and oven drying at 60 deg.C for 10 h. Taking 5g of the intercalation in a microwave oven, and carrying out microwave for 30s at 200W to obtain the expanded graphite. The expanded graphite was pressed into an expanded graphite preform at an extrusion rate of 0.2 which is an expansion rate. And (3) at the temperature of 45 ℃, immersing the compressed expanded graphite into molten paraffin with the phase transition temperature of 41 ℃, vacuumizing for 40min under the vacuum pressure of 82KPa, and immersing for 1.5h to obtain the phase transition composite material.
(2) Crushing the phase-change composite material, and then screening, wherein 100 parts by mass of a coarse component with the granularity range of 80-100 meshes and 22 parts by mass of a fine component with the granularity range of 500-700 meshes are taken;
(3) taking 15 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) as a binder, uniformly mixing, and dissolving in ethanol according to the mass fraction of 2.5%; taking 22 parts of fine components obtained by screening in the step (2), slowly adding an ethanol solution of a binder, and uniformly mixing;
(4) placing 100 parts of the coarse component obtained by screening in the step (2) in a coating dryer to be in a fluidized state, and spraying the liquid mixture obtained in the step (3) onto the surface of particles of the coarse component in the fluidized state at a speed of 250 ml/h; setting the air inlet temperature at 50 ℃, and drying for 2.5 hours to obtain the reshaped phase-change composite material.
(5) And (3) fully dissolving 7.5 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) in 2.5% of ethanol by mass fraction, spraying the two-component epoxy resin on the surface of the fluidized and shaped particles in the step (3) at a spraying speed of 250ml/h, setting the air inlet temperature to be 50 ℃, drying the materials while spraying, and drying for 105min to obtain the final product.
Example 3
(1) The expanded graphite/paraffin phase-change composite material is obtained by adopting a Chinese patent CN1294229C infiltration method: 30g of flake graphite with the fineness of 50 meshes and the carbon content of 94 percent, 300g of sulfuric acid with the concentration of 98 percent and 20g of potassium permanganate are taken and evenly stirred. Stirring at 45 deg.C and 300RPM for 30min, washing with water, filtering until the final solution has a pH of 4, and oven drying at 60 deg.C for 10 h. Taking 5g of the intercalation in a microwave oven, and carrying out microwave for 30s at 200W to obtain the expanded graphite. The expanded graphite was pressed into an expanded graphite preform at an extrusion rate of 0.2 which is an expansion rate. And (3) at the temperature of 50 ℃, immersing the compressed expanded graphite into molten paraffin with the phase transition temperature of 44 ℃, vacuumizing for 40min under the vacuum pressure of 82KPa, and immersing for 1.5h to obtain the phase transition composite material.
(2) Crushing the phase-change composite material, and then screening, wherein 100 parts by mass of a coarse component with a granularity range of 80-100 meshes and 20 parts by mass of a fine component with a granularity range of 400-500 meshes are taken;
(3) taking 15 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) as a binder, uniformly mixing, dissolving the mixture in ethanol according to the mass fraction of 5%, taking 20 parts of fine components obtained by screening in the step (2), slowly adding the ethanol solution of the binder, and uniformly mixing;
(4) placing 100 parts of the coarse component obtained by screening in the step (2) in a coating dryer to be in a fluidized state, and spraying the liquid mixture obtained in the step (3) onto the surface of particles of the coarse component in the fluidized state at a speed of 150 ml/h; setting the air inlet temperature at 50 ℃, and drying for 3.5h to obtain the shaped phase-change composite material.
(5) And (3) fully dissolving 7 parts of two-component epoxy resin (E51: JH-593 weight ratio is 3:1) in ethanol according to the mass fraction of 4.5%, spraying the two-component epoxy resin on the surface of the fluidized shaped particles in the step (3) at the spraying speed of 200ml/h, setting the air inlet temperature to be 50 ℃, drying the materials while spraying, and drying for 90min to obtain the final product.
Example 4
(1) The expanded graphite/paraffin phase-change composite material is obtained by adopting a Chinese patent CN1294229C infiltration method: 30g of flake graphite with the fineness of 50 meshes and the carbon content of 94 percent, 300g of sulfuric acid with the concentration of 98 percent and 20g of potassium permanganate are taken and evenly stirred. Stirring at 45 deg.C and 300RPM for 30min, washing with water, filtering until the final solution has a pH of 4, and oven drying at 60 deg.C for 10 h. Taking 5g of the intercalation in a microwave oven, and carrying out microwave for 30s at 200W to obtain the expanded graphite. The expanded graphite was pressed into an expanded graphite preform at an extrusion rate of 0.2 which is an expansion rate. And (3) immersing the compressed expanded graphite into molten paraffin with the phase transition temperature of 51.4 ℃ at 55 ℃, vacuumizing for 40min under the vacuum pressure of 82KPa, and immersing for 1.5h to obtain the phase transition composite material.
(2) Crushing the phase-change composite material, and then screening, wherein 100 parts by mass of coarse components with the granularity range of 60-80 meshes and 25 parts by mass of fine components with the granularity range of 700-800 meshes are taken;
(3) taking 15 parts of phenolic resin, dissolving the phenolic resin in ethanol according to the mass fraction of 3%, taking 25 parts of fine components obtained by screening in the step (2), slowly adding an ethanol solution of a binder, and uniformly mixing;
(4) placing 100 parts of the coarse component obtained by screening in the step (2) in a coating dryer to be in a fluidized state, and spraying the liquid mixture obtained in the step (3) onto the surface of particles of the coarse component in the fluidized state at a speed of 350 ml/h; setting the air inlet temperature at 60 ℃, and drying for 4h to obtain the shaped phase-change composite material.
(5) And (3) fully dissolving 6.5 parts of phenolic resin in 3.5% of ethanol by mass, spraying the phenolic resin on the surface of the shaped particles in the fluidized state in the step (3) at a spraying speed of 150ml/h, setting the air inlet temperature to be 60 ℃, drying the materials while spraying, and drying for 75min to obtain the final product.
The particles obtained in the examples were tested for stability, i.e. leak rate: and (4) testing the phase transition temperature by keeping the temperature for 20 hours at the temperature of 25 ℃ above, and testing the mass change of the phase transition temperature.
The properties are shown in the following table:
Claims (1)
1. a method for surface treatment of phase change composite particles, characterized by comprising the steps of:
(1) crushing and screening the expanded graphite/paraffin phase-change composite material, and taking 100 parts by mass of a coarse component of the phase-change composite material with the granularity range of 40-100 meshes and 15-40 parts by mass of a fine component of the phase-change composite material with the granularity range of 300-800 meshes;
(2) dissolving 10-30 parts by mass of a binder in 2-5% of ethanol, weighing the 800-mesh fine component obtained in the step (1), slowly adding an ethanol solution of the binder, and uniformly mixing to obtain a liquid mixture; the adhesive is two-component epoxy resin, E51: JH-593 weight ratio =3: 1;
(3) placing the coarse components of the phase-change composite material with 40-100 meshes obtained in the step (1) into a multifunctional coating dryer to be in a fluidized state, spraying the liquid mixture obtained in the step (2) onto the surfaces of fluidized particles, and drying the material while spraying, wherein the spraying conditions are as follows: the spraying speed of the liquid mixture is 150-350 ml/h; setting the air inlet temperature to be 5-15 ℃ higher than the phase change temperature, and drying for 1-4h to obtain shaped phase change composite particles;
(4) and (3) fully dissolving 5-8 parts of insulating resin in 2-5% mass fraction in ethanol, wherein the insulating resin and the binder in the step (2) are made of the same resin, the insulating resin ethanol solution is sprayed on the surface of the fluidized and shaped particles in the step (3), the material is dried while spraying, the spraying speed of the insulating resin ethanol solution is 100-250ml/h, the spraying drying temperature is 5-15 ℃ higher than the phase transition temperature, and the drying time is 1-2h, and finally the product is obtained.
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