CN107033851A - A kind of method of phase change composite material particle surface processing - Google Patents
A kind of method of phase change composite material particle surface processing Download PDFInfo
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- CN107033851A CN107033851A CN201710329109.3A CN201710329109A CN107033851A CN 107033851 A CN107033851 A CN 107033851A CN 201710329109 A CN201710329109 A CN 201710329109A CN 107033851 A CN107033851 A CN 107033851A
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- phase change
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
A kind of method of phase change composite material particle surface processing is the thick component of phase change composite material that the mesh of granularity 40 100 is taken to expanded graphite/wax phase change composite, granularity is mixed after the thin component of 300 800 purposes is added into the ethanol solution of binding agent for the thin component of phase change composite material of 300 800 mesh, obtains liquefied mixture；The thick component of the purpose of step 40 100 is placed in Multifunctional coating drying machine, it is at fluidizing state, liquefied mixture is sprayed into the particle surface of fluidisation state, dry materials while spraying, insulating resin is dissolved in ethanol, particle surface after shaping of the spraying in fluidisation state, material obtains drying while spraying, finally obtains product.The present invention has the advantages that stability is good, thermal conductivity factor is high, good sphericity, surface insulation.
Description
Technical field
The invention belongs to phase-change material technical field, and in particular to a kind of side of phase change composite material particle surface processing
Method.
Background technology
Phase-change material realizes temperature control purpose by the way that heat is discharged or absorbed during phase transition (solid-liquid).Phase transformation
Technology is without additional energy source and temperature-controlled precision is higher, is favored in increasing field.Conventional phase-change material has
Organic phase change material and inorganic hydrous salt phase transition material, inorganic hydrous salt phase transition material degree of supercooling are higher, rotten to metal material
Corrosion is stronger, and the organic phase change material phase transition temperature by representative of paraffin is adapted to, degree of supercooling is low, thus is increasingly becoming phase transformation
The preferred material of Material Field.In order to ensure the integrality of material shape or structure, phase-change material needs to carry out with framework material
It is compound, so as to avoid phase change material from being leaked in phase transition process.Method conventional at present is that paraffin is prepared into phase transformation is micro-
Capsule uses expanded graphite Adsorption Paraffin, to solve the leakage problem of phase-change material in energy storage-exergonic process.Chinese patent
CN106433567A reduces paraffin in phase transition process due to Volume Changes by coating two layers of resin in emulsion paraffin surface
Caused inelastic deformation.Expanded graphite compression is obtained compression-expansion stone by Chinese patent CN1294229C by piston press
Paraffin, is adsorbed in expanded graphite by ink by common or vacuum infiltration, largely solves paraffin in phase transition process
In leakage problem.
One of the problem of must being solved in the application of phase-change material and extension process is the heat transfer property and stably of material
Property (leakage) problem.Current microencapsulation material, nucleome is heat conductivility very low paraffin, and housing is also that heat conductivility is poor
Resin material.Thus the heat conductivility of the phase change composite material prepared is also relatively more general, while microcapsules are core shell structure,
Inside is all made up of paraffin, because Volume Changes can produce larger stress in phase transition process, so as to cause opening for housing
Split or damaged.The heat conduction of expanded graphite/paraffin phase change material and stability are relatively better, need to be broken in some application scenarios
It is combined after broken, but broken rear grain shape is complicated, sphericity is poor, is unfavorable for outer layer coating insulation and closest packing is multiple
Close, limit it and need to have the application of the occasion of heat conduction and insulation at some.
The content of the invention
It is an object of the invention to provide a kind of stability is good, thermal conductivity factor is high, the phase transformation of good sphericity, surface insulation is combined
The method of material granule surface treatment.
To achieve these goals, the method that the present invention is provided comprises the following steps：
(1) sieved after expanded graphite/wax phase change composite is crushed, take the phase that particle size range is 40-100 mesh
The thick constituent mass of change composite material is 100 parts, and particle size range is that the thin constituent mass of phase change composite material of 300-800 mesh is 15-
40 parts；
(2) quality is dissolved in after ethanol for 10-30 parts of binding agent with 2-5% mass fraction, weighed in step (1)
The thin component of 300-800 purposes, is slowly added to mix after the ethanol solution of binding agent, obtains liquefied mixture；
(3) the thick component of phase change composite material that 40-100 mesh is obtained in step (1) is placed in Multifunctional coating drying machine,
It is at fluidizing state, the liquefied mixture that step (2) is obtained is sprayed into the particle surface of fluidisation state, material while spraying
Dry；
(4) 5-8 parts of insulating resin is fully dissolved in ethanol with 2-5% mass fraction, be sprayed into step (3)
Particle surface after shaping in fluidisation state, material obtains drying while spraying, finally obtains product.
Expanded graphite/wax phase change composite as described above is obtained using Chinese patent CN1294229C infiltration process
Phase change composite material.
Binding agent as described above is thermosetting epoxy resin or phenolic resin etc.；
The condition of step (3) spraying is as described above：The spraying rate 150-350ml/h of liquefied mixture；Air intake is set
Temperature is, higher than 5-15 DEG C of phase transition temperature, the phase change composite material particle after shaping to be obtained after drying 1-4h.
The spraying conditions of step (4) as described above are：The spraying rate of insulating resin ethanol solution is 100-250ml,
The drying temperature of spraying is that drying time is 1-2h, obtains final products higher than 5-15 DEG C of phase transition temperature.
The binding agent that common coating is used is acrylic resin, hydroxymethyl cellulose etc., and heat resistance is poor, and
Belong to thermoplastic resin, volume is changed greatly before and after the phase-change material phase transformation used of the invention, therefore at relatively high temperatures, heat
Plastic resin can be deformed or even is bursting at the collision, and its resin does not have the effect of stability.Therefore the present invention uses thermosetting resin ring
Oxygen tree fat or phenolic resin, under higher temperature in use, also keep a hard form, improve its stability.
Coarse granule of the present invention is 40-100 mesh, and fine grained is 300-800 mesh.Because phase change grains are by machinery
Broken to obtain, surface topography is poor, and shape degree of profile is high.So if fine grain diameter is excessive, necessarily cause after shaping
Not only particle diameter becomes big to grain, and gap is larger between particle, therefore the fine grained diameter used is less than 300 mesh.The micropore of expanded graphite
Structure is general at 10-15 μm or so, thus adsorbs phase-change material, when particle diameter is near micro-pore diameter, micropore
It is easy to occur destruction to cause adsorption capacity to decline, therefore fine grained diameter is greater than 800 mesh.
The binding agent and insulating resin that the present invention is used are dissolved in the concentration of ethanol for 2-5wt%, when concentration is less than 2wt%,
Coating speed is too slow, less efficient.The roadmap of the present invention is, to coarse granule spray solution, to remove molten during fluidisation state
While agent, binding agent solidifies；When concentration is more than 5wt%, surface is coated between the particle of binding agent in fluidisation shape
Easily sticked together under the collision situation of state.
The spraying rate of step (3) of the present invention is 150-350ml/h, and during less than 150ml/h, disposal ability is relatively low, efficiency
It is low；When spraying rate is more than 350ml/h, the fine grained solution on coarse granule surface is more, and resin curing time is elongated, coarse granule
Adhesion phenomenon can be caused by being collided in fluid mapper process.
The spraying rate of step (4) of the present invention is 100-250ml/h, compared to step (3), the specific surface area of its particle than
Step (3) is medium and small, it is therefore desirable to reduce spraying rate, and spraying rate is excessive, and resin has little time to be fully cured so that between particle
Being collided in fluid mapper process causes adhesion.
EAT range of choice in step (3) of the present invention, (4) spraying process is higher than 5-15 DEG C of phase transition temperature.When
When EAT is less than 5 DEG C with the phase transition temperature temperature difference, not only treatment effeciency is caused to reduce, and the solidification of resin can be influenceed to cause to glue
Even.When EAT and phase transition temperature difference are more than 15 DEG C, although hot blast is short with particle contact time, and particle surface temperature may
Less than set temperature, but EAT it is too high can make phase-change material particle surface temperature be more than phase transition temperature so that undergo phase transition
Cause leakage.
The binding agent and dielectric resin material used in the step (3) and step (4) of the present invention is same resin, identical
Resin between compatibility it is relatively good, be conducive to keep material globality, will not after multiple thermal cycle between nucleocapsid occur
It is separated.
The present invention has the following advantages compared with prior art：
1. compared with surface shaping or paraffin systems microcapsules are not carried out, the expansion stone that thus method surface treatment is obtained
The stability of ink/wax phase change particle more preferably, the slip of general phase change composite material in 8-15%, and what the present invention was obtained
The slip of phase change composite material can reach 0.89%；The thermal conductivity factor of general phase-change microcapsule is less than 0.4W/mK, and surface
The expanded graphite phase change composite material Particle Thermal Conductivity of shaping is 12-15W/mK, and its thermal conductivity factor is after surface treatment
8-11W/m·K.Illustrate that the phase transformation composite particles thermal conductivity ratio paraffin microcapsule system after surface treatment is much higher, than processing
Preceding heat conductivility loss is less.
2. compared with general expanded graphite/wax phase change composite particles, the phase change composite material that prior art is obtained exists
On the premise of small range loss heat conductivility, its sphericity can be improved to 0.75 even more high, higher sphericity by 0.51
Outer layer insulation is more beneficial for, and subsequently the closest packing during heat conduction formed product is combined.
3. the expanded graphite not being surface-treated/wax phase change composite particles have good electric conductivity, limit
Its application in electronic applications.And the phase transformation composite particles for carrying out surface Shape correction and secondary surface insulation processing can be with
Completely insulated performance is reached, the field being had higher requirements simultaneously to heat conduction and insulation is can apply to.
Brief description of the drawings
Fig. 1 is the schematic diagram for the intermediate product particles that step of the present invention (3) is obtained；
Fig. 2 is the shape appearance figure (b) of broken rear (a) of expanded graphite/wax phase change composite and product of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail to the present invention, but do not constitute and the present invention is appointed
What is limited
Embodiment 1
(1) expanded graphite/wax phase change composite is obtained using Chinese patent CN1294229C infiltration process：Take fineness
The crystalline flake graphite 30g for being 94% for 50 mesh, carbon content, the sulfuric acid 300g of concentration 98%, potassium permanganate 20g are stirred evenly.45℃、
300RPM, which is persistently stirred, to be washed after 30min, filters, to the last solution PH=4, by filtrate in drying 10h at 60 DEG C.
Taking 5g intercalation things, microwave 30s obtains expanded graphite under 200W in micro-wave oven.Using press ratio as expansion rate 0.2 by expanded graphite
It is pressed into expanded graphite precast body.At 45 DEG C, compression-expansion graphite is immersed in the melt paraffin that phase transition temperature is 39 DEG C, with
82KPa vacuum pressure vacuumizes 40min, immersion 1.5h and obtains phase change composite material.
(2) sieved after phase change composite material is crushed, it is that the thick constituent mass of 40-60 purposes is 100 to take particle size range
Part, particle size range is that the thin constituent mass of 300-500 purposes is 18 parts；
(3) 10 parts of bicomponent epoxy resin (E51 is taken：JH-593 weight ratio=3:1) it is binding agent, is pressed after mixing
3wt% mass fraction is dissolved in after ethanol；The thin component for taking 18 parts of step (2) screenings to obtain, is slowly added to binding agent
Mixed after ethanol solution, obtain liquefied mixture；
(4) the thick component for obtaining 100 parts of step (2) screenings, which is placed in lagging cover drier, is at fluidizing state, will walk
Suddenly the liquefied mixture that (3) are obtained is with 200ml/h velocity spray to the thick component particles surface for fluidizing state；EAT is set
For 45 DEG C, the phase change composite material obtained after shaping for 2 hours is dried.
(5) by 5 parts of bicomponent epoxy resin (E51：JH-593 weight ratio=3:1) with 5% mass fraction in ethanol
In fully dissolve, with 125ml/h spraying rate be sprayed into step (3) in fluidisation state shaping after particle surface, if
EAT is put for 45 DEG C, material obtains drying while spraying, final products are obtained after drying 1h.
Embodiment 2
(1) expanded graphite/wax phase change composite is obtained using Chinese patent CN1294229C infiltration process：Take fineness
The crystalline flake graphite 30g for being 94% for 50 mesh, carbon content, the sulfuric acid 300g of concentration 98%, potassium permanganate 20g are stirred evenly.45℃、
300RPM, which is persistently stirred, to be washed after 30min, filters, to the last solution PH=4, by filtrate in drying 10h at 60 DEG C.
Taking 5g intercalation things, microwave 30s obtains expanded graphite under 200W in micro-wave oven.Using press ratio as expansion rate 0.2 by expanded graphite
It is pressed into expanded graphite precast body.At 45 DEG C, compression-expansion graphite is immersed in the melt paraffin that phase transition temperature is 41 DEG C, with
82KPa vacuum pressure vacuumizes 40min, immersion 1.5h and obtains phase change composite material.
(2) sieved after phase change composite material is crushed, it is that the thick constituent mass of 80-100 purposes is 100 to take particle size range
Part, particle size range is that the thin constituent mass of 500-700 purposes is 22 parts；
(3) 15 parts of bicomponent epoxy resin (E51 is taken：JH-593 weight ratio=3:1) it is binding agent, is pressed after mixing
2.5% mass fraction is dissolved in after ethanol；The thin component for taking 22 parts of step (2) screenings to obtain, is slowly added to binding agent
Mixed after ethanol solution；
(4) the thick component for obtaining 100 parts of step (2) screenings, which is placed in lagging cover drier, is at fluidizing state, will walk
Suddenly the liquefied mixture that (3) are obtained is with 250ml/h velocity spray to the thick component particles surface for fluidizing state；EAT is set
For 50 DEG C, the phase change composite material obtained after shaping for 2.5 hours is dried.
(5) by 7.5 parts of bicomponent epoxy resin (E51：JH-593 weight ratio=3:1) existed with 2.5% mass fraction
Fully dissolved in ethanol, the particle table after the shaping in fluidisation state in step (3) is sprayed into 250ml/h spraying rate
Face, it is 50 DEG C to set EAT, and material obtains drying while spraying, and final products are obtained after drying 105min.
Embodiment 3
(1) expanded graphite/wax phase change composite is obtained using Chinese patent CN1294229C infiltration process：Take fineness
The crystalline flake graphite 30g for being 94% for 50 mesh, carbon content, the sulfuric acid 300g of concentration 98%, potassium permanganate 20g are stirred evenly.45℃、
300RPM, which is persistently stirred, to be washed after 30min, filters, to the last solution PH=4, by filtrate in drying 10h at 60 DEG C.
Taking 5g intercalation things, microwave 30s obtains expanded graphite under 200W in micro-wave oven.Using press ratio as expansion rate 0.2 by expanded graphite
It is pressed into expanded graphite precast body.At 50 DEG C, compression-expansion graphite is immersed in the melt paraffin that phase transition temperature is 44 DEG C, with
82KPa vacuum pressure vacuumizes 40min, immersion 1.5h and obtains phase change composite material.
(2) sieved after phase change composite material is crushed, it is that the thick constituent mass of 80-100 purposes is 100 to take particle size range
Part, particle size range is that the thin constituent mass of 400-500 purposes is 20 parts；
(3) 15 parts of bicomponent epoxy resin (E51 is taken：JH-593 weight ratio=3:1) it is binding agent, 5% is pressed after mixing
Mass fraction be dissolved in after ethanol, the thin component for taking the screening of 20 parts of steps (2) to obtain is slowly added to the ethanol solution of binding agent
After mix；
(4) the thick component for obtaining 100 parts of step (2) screenings, which is placed in lagging cover drier, is at fluidizing state, will walk
Suddenly the liquefied mixture that (3) are obtained is with 150ml/h velocity spray to the thick component particles surface for fluidizing state；EAT is set
For 50 DEG C, the phase change composite material after shaping is obtained after drying 3.5h.
(5) by 7 parts of bicomponent epoxy resin (E51：JH-593 weight ratio=3:1) with 4.5% mass fraction in second
Fully dissolved in alcohol, the particle surface after the shaping in fluidisation state in step (3) be sprayed into 200ml/h spraying rate,
It is 50 DEG C to set EAT, and material obtains drying while spraying, and final products are obtained after drying 90min.
Embodiment 4
(1) expanded graphite/wax phase change composite is obtained using Chinese patent CN1294229C infiltration process：Take fineness
The crystalline flake graphite 30g for being 94% for 50 mesh, carbon content, the sulfuric acid 300g of concentration 98%, potassium permanganate 20g are stirred evenly.45℃、
300RPM, which is persistently stirred, to be washed after 30min, filters, to the last solution PH=4, by filtrate in drying 10h at 60 DEG C.
Taking 5g intercalation things, microwave 30s obtains expanded graphite under 200W in micro-wave oven.Using press ratio as expansion rate 0.2 by expanded graphite
It is pressed into expanded graphite precast body.At 55 DEG C, compression-expansion graphite is immersed in the melt paraffin that phase transition temperature is 51.4 DEG C, with
82KPa vacuum pressure vacuumizes 40min, immersion 1.5h and obtains phase change composite material.
(2) sieved after phase change composite material is crushed, it is that the thick constituent mass of 60-80 purposes is 100 to take particle size range
Part, particle size range is that the thin constituent mass of 700-800 purposes is 25 parts；
(3) 15 parts of phenolic resin is taken, ethanol is dissolved in by 3% mass fraction, take that 25 parts of steps (2) screenings obtain is thin
Component, is slowly added to mix after the ethanol solution of binding agent；
(4) the thick component for obtaining 100 parts of step (2) screenings, which is placed in lagging cover drier, is at fluidizing state, will walk
Suddenly the liquefied mixture that (3) are obtained is with 350ml/h velocity spray to the thick component particles surface for fluidizing state；EAT is set
For 60 DEG C, the phase change composite material after shaping is obtained after drying 4h.
(5) by 6.5 parts of phenolic resin, fully dissolved in ethanol with 3.5% mass fraction, with 150ml/h spray
Apply velocity spray into step (3) in fluidisation state shaping after particle surface, set EAT be 60 DEG C, spraying it is same
When material obtain drying, obtain final products after drying 75min.
Embodiment is obtained into particle and does the i.e. slip test of stability：More than phase transition temperature it is incubated 20 hours under the conditions of 25 DEG C
Test, tests its mass change.
Its performance is as shown in the table：
Claims (4)
1. a kind of method of phase change composite material particle surface processing, it is characterised in that comprise the following steps：
（1）Sieved after expanded graphite/wax phase change composite is crushed, take the phase transformation that particle size range is 40-100 mesh to answer
The thick constituent mass of condensation material is 100 parts, and particle size range is that the thin constituent mass of phase change composite material of 300-800 mesh is 15-40 parts；
（2）Quality is dissolved in after ethanol for 10-30 parts of binding agent with 2-5% mass fraction, step is weighed（1）Middle 300-
The thin component of 800 purposes, is slowly added to mix after the ethanol solution of binding agent, obtains liquefied mixture；
（3）By step（1）In obtain the thick component of phase change composite material of 40-100 mesh and be placed in Multifunctional coating drying machine, make it
In fluidisation state, by step（2）Obtained liquefied mixture is sprayed into the particle surface of fluidisation state, and material is done while spraying
It is dry；
（4）5-8 parts of insulating resin is fully dissolved in ethanol with 2-5% mass fraction, step is sprayed into（3）In be in
The particle surface after the shaping of state is fluidized, material obtains drying while spraying, finally obtains product.
2. the method for a kind of phase change composite material particle surface processing as claimed in claim 1, it is characterised in that described
Binding agent be thermosetting epoxy resin or phenolic resin.
3. a kind of method of phase change composite material particle surface processing, it is characterised in that the step（3）The condition of spraying is：Liquid
The spraying rate 150-350ml/h of state mixture；It is, higher than 5-15 DEG C of phase transition temperature, to be obtained after drying 1-4h to set EAT
Phase change composite material particle after shaping.
4. a kind of method of phase change composite material particle surface processing, it is characterised in that described step（4）Spraying conditions be：
The spraying rate of insulating resin ethanol solution is 100-250ml, and the drying temperature of spraying is, higher than 5-15 DEG C of phase transition temperature, to dry
Time is 1-2h.
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| CN114381237A (en) * | 2022-01-07 | 2022-04-22 | 瑞声科技（南京）有限公司 | Heat storage composite material and preparation method thereof |
| CN115870493A (en) * | 2023-03-01 | 2023-03-31 | 矿冶科技集团有限公司 | Low-burning-loss composite powder and preparation method thereof |
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| CN107033851B (en) | 2020-09-22 |
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