CN108774500A - A kind of fast preparation method of paraffin graphite phase change composite material - Google Patents
A kind of fast preparation method of paraffin graphite phase change composite material Download PDFInfo
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- CN108774500A CN108774500A CN201810943701.7A CN201810943701A CN108774500A CN 108774500 A CN108774500 A CN 108774500A CN 201810943701 A CN201810943701 A CN 201810943701A CN 108774500 A CN108774500 A CN 108774500A
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- 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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Abstract
The present invention relates to a kind of fast preparation methods of paraffin graphite phase change composite material.It includes the following steps that heating paraffin is fused into liquid, 92-140 DEG C will be heated in natural flake graphite by step 1 heating；Step 2 is mixed, and the natural flake graphite in step 1 is added in the vasoliniment in step 1, is by weight percentage the ratio mixing that 20-45% natural flake graphites and weight percent are 55-80% paraffin, then stirs to get graphite paraffin mixture;Step 3 cools down, and the graphite paraffin mixed material in step 2 is cooled to 42-90 DEG C；Graphite paraffin mixture in step 4 is packed into compression moulding and pressurize in the mold of preheating by step 4 compression moulding；Step 5 depanning, while hot depanning obtain paraffin graphite phase change composite material.In preparation process of the present invention, it is only necessary in proportion after evenly mixing by the phase change paraffin of heating fusing and natural flake graphite, can be obtained paraffin graphite phase change composite material through compression molding, the production cycle greatly shortens.
Description
Technical field
The present invention relates to the technical field of paraffin graphite phase change composite material, especially a kind of paraffin graphite phase transformation composite wood
The fast preparation method of material.
Background technology
During the storage of thermal energy and utilization, it is usually present supply time and spatially unmatched contradiction, such as sun
Can intermittence, the peak-valley difference of electric load, periodic duty great-power electronic radiating element heat dissipation and industrial exhaust heat profit
With etc..Phase-changing energy storage material is to absorb or discharge amount of heat when undergoing phase transition by material to realize energy storage and utilization,
Energy supply and demand unmatched contradiction over time and space can effectively be solved.Phase-changing energy storage material can according to the variation pattern of phase
It is divided into solid-liquid phase change, four class of solid-solid phase-change, liquid-gas and solid-gas phase transformation.Two class materials have a large amount of gas in phase transition process afterwards
Body generates, volume change is very big, seldom uses in practical applications.Then there is phase transition temperature height, enthalpy of phase change in solid-solid phase transition material
The higher disadvantage of low and cost, application are also very limited.Solid-liquid phase change material is due to at low cost, latent heat of phase change
Greatly, transition temperature range is wide and without supercooling or many advantages, such as precipitation phenomenon, is the most a kind of phase of current domestic and international application
Become material.But it is low all to there is thermal conductivity in phase-changing energy storage material itself（Generally in 1W/m.K or less）, the problem of heat transfer property difference, this
Necessarily affect energy storage rate.Therefore, need to be compound by phase-changing energy storage material and the progress of the material of excellent thermal conductivity, to real
The purpose of augmentation of heat transfer is now carried out to phase-changing energy storage material.
For this purpose, many scientific workers are directed to the Material cladding of solid-liquid phase change material and excellent thermal conductivity both at home and abroad
Aspect has carried out a large amount of research work.By the preferable metallic particles of heat conductivility or powder（Such as Ag, Al and Cu powder）It is added to
It is a kind of method of relatively simple practicality to improve the heat conductivility of phase-change material in phase-change material.American scientist is in solar heat
It is found after Al powder is added in phase-changing energy storage material in hydrophone, when the mass content of Al powder reaches 50% or more, heat conduction efficiency
It improves nearly more than 4 times.Influence of the addition of American scientist system thinking Ag particles to phase-change material tetradecane heat conductivility.
Studies have shown that with the increase of Ag granular mass, the thermal coefficient of composite material improves, but the latent heat of material is caused to decline；This
Outside, since metal generally has higher density, the weight for causing entire hold over system increases, and practicability is deteriorated.It is new in recent years
A kind of material that type grows up is by the porous materials such as high-thermal conductive metal foam, graphite foam and expanded graphite and phase-change material
It is compound, to improve the thermal conductivity and heat exchange efficiency of phase-change material.But metal foaming material is perishable, density is high, and and phase transformation
Material compatibility is poor, to limit its application.The preferable porous carbon material of light and heat conductivility such as graphite foam, expansion stone
Many advantages, such as ink has that thermal conductivity is high, density is low, chemical stability is strong and is good with phase-change material compatibility, is phase-change material
Ideal storage carrier.Some researchers are prepared for paraffin/graphite foam phase change composite material using graphite foam Adsorption Paraffin.
The result shows that：The pore structure and thermal coefficient of graphite foam are an important factor for influencing final composite material hot property.With paraffin
Thermal coefficient（0.3W/m.K）It compares, the thermal coefficient of paraffin/graphite foam composite material improves nearly 50 times, up to
14.6 W/m.K.But graphite foam is generally through asphalt foaming, high pressure charing and high temperature graphitization（2500 DEG C or more）Etc. processes come
It is prepared, not only to equipment requirement height（High temperature and pressure）, the production cycle is long and high energy consumption（Cost is big）And it limits it and answers extensively
With.Some researchers also utilize compressible expanded graphite（CENG）For storage carrier, by the way of vacuum infiltration and phase transformation
The progress of material paraffin is compound, is prepared for paraffin/CENG composite materials.Compared with the thermal coefficient of paraffin, paraffin/CENG is compound
The thermal coefficient of material improves 25 times or more, but since the thermal coefficient of CENG itself is relatively low, the heat conduction of final composite material
Coefficient is limited in 50W/m.K hereinafter, it is difficult to meeting the requirement in some special heat-radiating fields.In addition, being prepared in CENG
In the process, raw materials used natural graphite must acidified, washing and high temperature puffing（900 DEG C or so）Etc. processes, not only production week
Phase is long and has large quantity of exhaust gas and waste water to generate, and causes seriously to pollute to environment.
Invention content
It is an object of the invention to overcome above-mentioned the shortcomings of the prior art, and provide a kind of simple and reasonable for structure, production
The fast preparation method for the paraffin graphite phase change composite material that period is short, environmentally friendly, manufacturing cost is low, heat transfer efficiency is high.
The object of the present invention is achieved like this：
A kind of fast preparation method of paraffin graphite phase change composite material, includes the following steps, step 1 heating, by heating paraffin
It is fused into liquid, and constant temperature will be heated to 92-140 DEG C to 92-140 DEG C in natural flake graphite；
Step 2 is mixed, and the natural flake graphite in step 1 is added in the vasoliniment in step 1, by weight hundred
Divide the ratio mixing that ratio is 20-45% natural flake graphites and weight percent is 55-80% paraffin, then stirs to get graphite stone
Wax mixture, mixing time 10-30min;
Step 3 cools down, and the graphite paraffin mixed material in step 2 is cooled to 42-90 DEG C；
Graphite paraffin mixture in step 4 is packed into compression moulding and pressurize in the mold of preheating by step 4 compression moulding,
The clamping pressure of mold is 200-500kg/cm2, and the preheating temperature of mold is 42-90 DEG C, dwell time 5-15min；
Step 5 depanning, after pressurize, depanning while hot obtains paraffin graphite phase change composite material.
The present invention can also improve further below.
The average particle size of the natural flake graphite is 75-380 μm, carbon content 96-99wt.%, and the paraffin melting point is
47-95 DEG C, molecular weight 254-506, molecular formula CnH2n+2, ranging from=18-36 of wherein n, the heat of fusion of paraffin（It is latent
Heat）For 140-280J/g.
Beneficial effects of the present invention are as follows：
（1）During material preparation of the present invention, it is only necessary to which the phase change paraffin of heating fusing and natural flake graphite is equal in proportion
After even mixing, paraffin graphite phase change composite material is can be obtained through compression molding, the production cycle greatly shortens.
（2）In addition, in existing paraffin/graphite foam phase change composite material and paraffin/CENG composite manufacturing process,
It is respectively necessary for by high temperature graphitization（2500 DEG C or more）And high temperature puffing（850~1050℃）Processing；And above-mentioned composite material is
By under high temperature, high pressure, the phase change paraffin after fusing is penetrated into the hole of graphite material using vacuum-pressure technique dipping
In, not only energy consumption is big, and also relatively high to equipment requirement so that production cost is larger.And prepared by the composite material of the present invention
In the process, it is not required to that material preparation can be completed by processes such as high temperature sintering and high-pressure impregnations（Maximum temperature is only 140 DEG C）, because
This energy consumption is smaller, and manufacturing cost is also greatly lowered.
（3）Moreover, for paraffin/graphite foam phase change composite material, due to it is raw materials used be pitch, in high-temperature process mistake
A large amount of hydrocarbons decompose volatilization, effusion in journey, cause environmental pollution；And in paraffin/CENG composite manufacturing process,
A large amount of spent acid and exhaust gas are will produce, will also be polluted the environment.It is used in composite material production preparation process in the present invention
Raw material natural flake graphite powder and the non-volatile object of phase change paraffin generate, therefore not will produce pollutant.
（4）More have plenty of, its heat conductivility of any kind of graphite material each depends on the orientation row of internal microstructure
Row degree.Graphite microcrystalline structure aligns that degree is higher, then the heat conductivility of material is better.Paraffin/CENG composite materials
In preparation process, raw materials used natural flake graphite is acidified, after high temperature puffing, and volume expansion is internal to 150 times or more
Graphite microcrystal orientation is destroyed, and Turbostratic is presented.Although crystallite orientation degree can be promoted once again in subsequent nipping process,
But it can not possibly be restored to the state of original natural flake graphite, therefore the thermal coefficient of final composite material is relatively low.And
It is prepared in composite material using present invention process, the intrinsic height-oriented knot of raw materials used natural flake graphite particle itself
Structure is not affected by destruction, from start to finish is kept；In addition, during hot-forming, natural flake graphite particle mutually it
Between along being aligned perpendicular to pressing direction, therefore the thermal coefficient of prepared paraffin graphite phase change composite material also compared with
Height is greatly improved its heat exchange efficiency in energy storage system.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1, the paraffin that weight percent is 60%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 95 DEG C；Paraffin melting point used in it is 50 DEG C, molecular weight 282, molecular formula C20H42, heat of fusion（Latent heat）
For 167J/g.After natural flake graphite is preheated to 95 DEG C in the heater, it is added to for 40% by weight percentage above-mentioned molten
In the vasoliniment of change, and be persistently stirred 15min, used in natural flake graphite average particle size be 350 μm, carbon
Content is 98.6 wt.%.After mixing, mixed material is cooled to 45 DEG C, is then loaded into the steel die of preheating, so
It is pressed under the pressure of 300kg/cm2 afterwards and pressurize 10min, wherein steel die preheating temperature is 45 DEG C.Pressurize
After, the preparation of paraffin graphite phase change composite material is completed in depanning while hot, and Fundamental Physical Properties are shown in Table 1.
Embodiment 2, the paraffin that weight percent is 66%, which is placed in heating in steel blending tank, makes its fusing, then constant temperature
To 117 DEG C；Paraffin melting point used in it is 72 DEG C, molecular weight 366, molecular formula C26H54, heat of fusion（Latent heat）For
194J/g.After natural flake graphite is preheated to 117 DEG C in the heater, it is added to for 34% by weight percentage above-mentioned molten
In the vasoliniment of change, and be persistently stirred 20min, used in natural flake graphite average particle size be 264 μm, carbon
Content is 96.8 wt.%.After mixing, mixed material is cooled to 67 DEG C, is then loaded into the steel die of preheating, so
It is pressed under the pressure of 360kg/cm2 afterwards and pressurize 8min, wherein steel die preheating temperature is 67 DEG C.Pressurize knot
The preparation of paraffin graphite phase change composite material is completed in Shu Hou, while hot depanning, and Fundamental Physical Properties are shown in Table 1.
Embodiment 3, the paraffin that weight percent is 75%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 130 DEG C；Paraffin melting point used in it is 85 DEG C, molecular weight 436, molecular formula C31H64, heat of fusion（Latent heat）
For 218J/g.After natural flake graphite is preheated to 130 DEG C in the heater, it is added to for 25% by weight percentage above-mentioned
In the vasoliniment of fusing, and be persistently stirred 16min, used in natural flake graphite average particle size be 206 μm,
Carbon content is 99 wt.%.After mixing, mixed material is cooled to 80 DEG C, is then loaded into the steel die of preheating, so
It is pressed under the pressure of 200kg/cm2 afterwards and pressurize 5min, wherein steel die preheating temperature is 80 DEG C.Pressurize knot
The preparation of paraffin graphite phase change composite material is completed in Shu Hou, while hot depanning, and Fundamental Physical Properties are shown in Table 1.
Embodiment 4, the paraffin that weight percent is 75%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 137 DEG C；Paraffin melting point used in it is 92 DEG C, molecular weight 448, molecular formula C34H40, heat of fusion（Latent heat）
For 249J/g.After natural flake graphite is preheated to 137 DEG C in the heater, it is added to for 25% by weight percentage above-mentioned
In the vasoliniment of fusing, and be persistently stirred 15min, used in natural flake graphite average particle size be 264 μm,
Carbon content is 99 wt.%.After mixing, mixed material is cooled to 87 DEG C, is then loaded into the steel die of preheating, so
It is pressed under the pressure of 240kg/cm2 afterwards and pressurize 7min, wherein steel die preheating temperature is 87 DEG C.Pressurize knot
The preparation of paraffin graphite phase change composite material is completed in Shu Hou, while hot depanning, and Fundamental Physical Properties are shown in Table 1.
Embodiment 5, the paraffin that weight percent is 55%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 97 DEG C；Paraffin melting point used in it is 52 DEG C, molecular weight 296, molecular formula C21H44, heat of fusion（Latent heat）
For 175J/g.After natural flake graphite is preheated to 87 DEG C in the heater, it is added to for 45% by weight percentage above-mentioned molten
In the vasoliniment of change, and be persistently stirred 20min, used in natural flake graphite average particle size be 280 μm, carbon
Content is 96.5 wt.%.After mixing, mixed material is cooled to 47 DEG C, is then loaded into the steel die of preheating, so
It is pressed under the pressure of 350kg/cm2 afterwards and pressurize 10min, wherein steel die preheating temperature is 47 DEG C.Pressurize
After, the preparation of paraffin graphite phase change composite material is completed in depanning while hot, and Fundamental Physical Properties are shown in Table 1.
Embodiment 6, the paraffin that weight percent is 55%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 97 DEG C；Paraffin melting point used in it is 52 DEG C, molecular weight 296, molecular formula C21H44, heat of fusion（Latent heat）
For 175J/g.After natural flake graphite is preheated to 97 DEG C in the heater, it is added to for 45% by weight percentage above-mentioned molten
In the vasoliniment of change, and be persistently stirred 20min, used in natural flake graphite average particle size be 80 μm, carbon
Content is 97 wt.%.After mixing, mixed material is cooled to 47 DEG C, is then loaded into the steel die of preheating, then
It is pressed under the pressure of 350kg/cm2 and pressurize 10min, wherein steel die preheating temperature is 47 DEG C.Pressurize knot
Beam completes the preparation of paraffin graphite phase change composite material or, depanning while hot, and Fundamental Physical Properties are shown in Table 1.
Embodiment 7, the paraffin that weight percent is 65%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 103 DEG C；Paraffin melting point used in it is 58 DEG C, molecular weight 310, molecular formula C22H46, heat of fusion（Latent heat）
For 184J/g.After natural flake graphite is preheated to 103 DEG C in the heater, it is added to for 35% by weight percentage above-mentioned
In the vasoliniment of fusing, and be persistently stirred 20min, used in natural flake graphite average particle size be 106 μm,
Carbon content is 97.5 wt.%.After mixing, mixed material is cooled to 53 DEG C, is then loaded into the steel die of preheating,
Then it is pressed under the pressure of 300kg/cm2 and pressurize 10min, wherein steel die preheating temperature is 53 DEG C.It protects
After pressure, the preparation of paraffin graphite phase change composite material is completed in depanning while hot, and Fundamental Physical Properties are shown in Table 1.
Embodiment 8, the paraffin that weight percent is 70%, which is placed in heating in steel blending tank, first makes its fusing, then
Constant temperature is to 112 DEG C；Paraffin melting point used in it is 67 DEG C, molecular weight 338, molecular formula C24H50, heat of fusion（Latent heat）
For 197J/g.After natural flake graphite is preheated to 103 DEG C in the heater, it is added to for 30% by weight percentage above-mentioned
In the vasoliniment of fusing, and be persistently stirred 16min, used in natural flake graphite average particle size be 142 μm,
Carbon content is 98.5 wt.%.After mixing, mixed material is cooled to 62 DEG C, is then loaded into the steel die of preheating,
Then it is pressed under the pressure of 250kg/cm2 and pressurize 10min, wherein steel die preheating temperature is 62 DEG C.It protects
After pressure, the preparation of paraffin graphite phase change composite material is completed in depanning while hot, and Fundamental Physical Properties are shown in Table 1.
The Fundamental Physical Properties that paraffin graphite phase change composite material is made in above example are listed in table 1：
The Fundamental Physical Properties parameter of 1 paraffin graphite phase change composite material of table
Remarks：
∥：It is parallel to graphite linings direction；
⊥：Perpendicular to graphite linings direction.
Claims (2)
1. a kind of fast preparation method of paraffin graphite phase change composite material, includes the following steps, step 1 heating, by paraffin plus
Hot melt chemical conversion liquid, and constant temperature will be heated to 92-140 DEG C to 92-140 DEG C in natural flake graphite；
Step 2 is mixed, and the natural flake graphite in step 1 is added in the vasoliniment in step 1, by weight hundred
Divide the ratio mixing that ratio is 20-45% natural flake graphites and weight percent is 55-80% paraffin, then stirs to get graphite stone
Wax mixture, mixing time 10-30min;
Step 3 cools down, and the graphite paraffin mixed material in step 2 is cooled to 42-90 DEG C；
Graphite paraffin mixture in step 4 is packed into compression moulding and pressurize in the mold of preheating by step 4 compression moulding,
The clamping pressure of mold is 200-500kg/cm2, and the preheating temperature of mold is 42-90 DEG C, dwell time 5-15min；
Step 5 depanning, after pressurize, depanning while hot obtains paraffin graphite phase change composite material.
2. the fast preparation method of paraffin graphite phase change composite material according to claim 1, characterized in that the natural squama
The average particle size of piece graphite is 75-380 μm, carbon content 96-99wt.%, and the paraffin melting point is 47-95 DEG C, and molecular weight is
The heat of fusion of ranging from=18-36 of 254-506, molecular formula CnH2n+2, wherein n, paraffin are 140-280J/g.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587339A (en) * | 2004-07-15 | 2005-03-02 | 同济大学 | Porous graphite base phase change energy storage composite material and its preparing method |
| CN103555282A (en) * | 2013-11-05 | 2014-02-05 | 中国科学院山西煤炭化学研究所 | Preparation method of high-heat-conductivity paraffin/graphite phase-change composite material |
| CN104877641A (en) * | 2015-05-28 | 2015-09-02 | 中国科学院山西煤炭化学研究所 | Method for low-cost quick preparation of paraffin/graphite phase-change composite material |
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- 2018-08-18 CN CN201810943701.7A patent/CN108774500A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587339A (en) * | 2004-07-15 | 2005-03-02 | 同济大学 | Porous graphite base phase change energy storage composite material and its preparing method |
| CN103555282A (en) * | 2013-11-05 | 2014-02-05 | 中国科学院山西煤炭化学研究所 | Preparation method of high-heat-conductivity paraffin/graphite phase-change composite material |
| CN104877641A (en) * | 2015-05-28 | 2015-09-02 | 中国科学院山西煤炭化学研究所 | Method for low-cost quick preparation of paraffin/graphite phase-change composite material |
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Application publication date: 20181109 |