CN100494306C - High heat conduction and figuration composite phase-changing material and preparation method thereof - Google Patents
High heat conduction and figuration composite phase-changing material and preparation method thereof Download PDFInfo
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- CN100494306C CN100494306C CNB2006100330469A CN200610033046A CN100494306C CN 100494306 C CN100494306 C CN 100494306C CN B2006100330469 A CNB2006100330469 A CN B2006100330469A CN 200610033046 A CN200610033046 A CN 200610033046A CN 100494306 C CN100494306 C CN 100494306C
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Abstract
The related preparation method for composite phase-change material with high heat conductivity and shaping comprises: adding the homogeneous AlN and carbowax powder into the silica sol; dripping accelerant, stirring to form three-dimensional network gel by sol-gel reaction; drying and mashing the gel into powder; dewatering, adding modifier in N2 protection at 120Deg. This product has high thermal conductivity, well forming property and stable performance, and fit to spread to electronic material and building trades.
Description
Technical field
The present invention relates to a kind of organism and composite material of inorganic matter, particularly a kind of high heat conduction and figuration composite phase-changing material.
The invention still further relates to the preparation method of described high heat conduction and figuration composite phase-changing material.
Background technology
Paraffin, stearic acid, polyoxyethylene glycol etc. have very high phase transformation enthalpy (more than the 170kJ/kg), have crucial application prospect as organic phase change material.But there is deficiency in actual applications in these materials:
(1) phase change material takes place in solid-liquid phase-change process in fusion, and liquid can leak out from system, needs special container to encapsulate, and this not only increases cost, and has increased the thermal resistance of heat-transfer medium and phase change material;
(2) organic phase change material heat conductivility poor (thermal conductivity is about 0.2W/mk) after phase-transition heat-storage, is difficult to fast energy transformation be gone out.
Add in the phase change material and support the setting composition and can solve its leakage problem preferably.Being divided into the have higher melt superpolymer of (exceeding 30~70 ℃ than phase change material invert point) owing to support to be shaped as, as high density polyethylene (HDPE) etc., or is resistant to elevated temperatures inorganic porous material, as expanded graphite etc.When taking place to change mutually, although phase change material shows as fused solution on microcosmic, but because the setting component is to its restriction, the profile that on macroscopic view, still can keep composite phase-change material, phase change material can therefrom not leak out yet, therefore phase change material can directly contact with heat-transfer medium, thereby can reduce cost, and improves heat exchange efficiency.The advantage that superpolymer is made the setting material is that shape stability is good, and easy characteristics such as processing, weak point are that life-time service can exist the aging and phase change material of base material problem such as to separate from the composition that formalizes; Expanded graphite is made the setting composition and is had characteristics such as porosity height, thermal conductivity is good, density is low, and the composite phase-change material thermal conductivity that obtains is good, and energy storage density is big, and weak point is to exist defectives such as compressive deformation and shape stability be relatively poor.
Add the high thermal conductivity filler and can improve the phase change material heat conductivility effectively.As add copper powder, aluminium powder and the metal oxide thereof etc. of high thermal conductivity, can significantly improve the thermal conductivity of composite phase-change material, increase thermal conversion efficiency, weak point is to exist nonisulated (conduction), not corrosion-resistant and differ bigger with phase change material density, easily layering, disperse unequal problem.
Summary of the invention
The present invention is directed to the defective that prior art exists, have thermal conductivity and shape stability is good, heat storage capacity is high, the high heat conduction and the figuration composite phase-changing material of stable performance machine-shaping but provide a kind of, can be applicable in industries such as electronic component heat controlled material, heat-accumulation temperature-adjustment textiles and building energy conservation bodies of wall.
Another object of the present invention is to provide the preparation method of described high heat conduction and figuration composite phase-changing material.
The preparation method of high heat conduction of the present invention and figuration composite phase-changing material comprises the steps:
(1) aluminium nitride powder and polyoxyethylene glycol powder are mixed, join in the silicon sol, drip promotor, stir, colloidal sol-gel reaction takes place, form the three-dimensional network gel;
(2), smash to pieces and obtain the gel powder with behind the three-dimensional network gel drying;
(3) the gel powder is removed moisture, under nitrogen protection and 120 ℃, adds properties-correcting agent.
The parts by weight of described each component are as follows:
Polyoxyethylene glycol 40~85
Promotor 0.01~0.1
Properties-correcting agent 0.1~1.5
The polyoxyethylene glycol number-average molecular weight is 1000~20000;
Described promotor is a kind of or more than one mixtures in magnesium chloride, calcium chloride, aluminum chloride, the Tai-Ace S 150;
Described properties-correcting agent is organo silane coupling agent; Preferred aminopropyl triethoxysilane (KH-550) and/or glycidyl ether oxygen propyl trimethoxy silicane (KH-560).
High heat conduction that obtains and figuration composite phase-changing material can also be 60~120 ℃ in temperature, and pressure is that 5~25Mpa compressing tablet makes block;
Wherein the preferred weight umber of aluminium nitride, silicon sol, promotor, properties-correcting agent is as follows:
Promotor 0.01~0.03
Properties-correcting agent 0.5~1.0
In the described step (1), the molecular weight polyethylene glycol scope be 3000~6000 with the molecular weight polyethylene glycol scope be 10000~20000 better by 0.5~1/1 composite effect.
In the described step (1), the particle size range of aluminium nitride powder is that 0.5~5 μ m, crystal formation are α, β type, and is composite by the aluminium nitride powder of different-grain diameter, different crystal forms, the high heat conduction that makes, the inorganic-organic composite phase-change material better performances of setting.Press α type aluminium nitride/β type aluminium nitride=1/2, size and weight ratio thereof are respectively by 0.5~1.0/3.0~5.0 μ m, 3/1 composite best results.
In the step (2), the forced air drying in 80 ℃ of baking ovens of three-dimensional network gel can be cooled to room temperature after 24~48 hours, take out to smash to pieces and to stir and obtain the gel powder;
In the step (3), the gel powder can be vacuumized under 40 ℃ 2~4 hours, remove moisture.
Ultimate principle of the present invention is: the mineral filler aluminium nitride, have high thermal conductivity, high temperature resistant, corrosion-resistant, the insulation non-conductive, thermal expansivity is little, characteristics such as its density and organic phase change material are suitable, when a certain proportion of aluminium nitride is dispersed in the phase change material, owing to " series connection " effect between aluminum nitride particle, can improve the thermal conductivity of composite phase-change material, but and the interior coefficient of thermal expansion that reduces composite phase-change material of certain limit.
The polarity of the terminal hydroxy group of polyoxyethylene glycol makes its dissolving easily in silicon sol, colloidal sol-gel reaction by silicon sol, can make the each component homodisperse, obtain high-specific surface area, microporous reticulated structure silicon-dioxide simultaneously, because the capillary adsorption can be adsorbed in the hydrophilic polyglycol phase change material in the stephanoporate framework of silicon-dioxide; Moreover, the silicon hydroxyl of silica sphere (Si-OH) and polyoxyethylene glycol terminal hydroxy group (CH
2-form stronger hydrogen bond between OH), further strengthened both interactions, thereby polyoxyethylene glycol can be embedded into firmly in the network of silica, solid when taking place-during liquid phase transition, the polyoxyethylene glycol liquid that can not leaks out from skeleton.After polyoxyethylene glycol dissolved in silicon sol, because the relative stability of silicon sol, colloidal sol-gel reaction speed was very slow, needed to add promotor such as soluble metal high price salt destruction colloidal sol electrostatic double layer, impelled the generation of matrix material gel.In addition, polar group---hydroxyl is arranged owing to powder surface is remaining, very sensitive to airborne moisture, need to add silane coupling agent to remove activity hydroxy to show its hydrophobic performance.
Compared with prior art, the material that obtains of the present invention has following advantage and effect:
(1) the latent heat amount is big, accumulation of energy is effective;
(2) thermal conductivity is good, helps the transmission and the conversion of heat;
(3) the setting performance is good, and the effect that formalizes is preferably just arranged when support matrix content 10%;
(4) stability is high.Because aluminium nitride, silicon-dioxide are high temperature resistant, corrosion-resistant, low thermal coefficient of expansion component, stability itself is strong, with polyoxyethylene glycol when composite, because of capillary absorption and hydrogen bond action, increased pining down mutually of the two, and adopted colloidal sol-gel process, its component is uniformly dispersed.
Description of drawings
Fig. 1 is the thermal conductivity comparison diagram of composite phase-change material of the present invention and other phase change materials;
Fig. 2 is the polarizing microscope figure of polyoxyethylene glycol and high heat conduction of the present invention and figuration composite phase-changing material, wherein: Fig. 2 (a), 2 (b), 2 (c) are respectively the polarized light microscopy figure of pure polyoxyethylene glycol in the time of 60 ℃, 64 ℃, 68 ℃, and Fig. 2 (d) is high heat conduction, the polarized light microscopy figure of the inorganic-organic composite phase-change material of setting under 60 ℃~110 ℃ range of temperature;
Fig. 3 is the transmission electron microscope picture (embodiment 1) of high heat conduction of the present invention and figuration composite phase-changing material;
Fig. 4 is the DSC curve (embodiment 1) of high heat conduction of the present invention and figuration composite phase-changing material;
Of the present invention high heat conduction that Fig. 5 obtains for embodiment 1,2,3 and figuration composite phase-changing material at different pressures condition lower sheeting thermal conductivity test pattern.
Embodiment
Embodiment 1
(1) under the room temperature, add 600g polyoxyethylene glycol powder (polyoxyethylene glycol 5000 and cetomacrogol 1000 0 mix by 1/2) in the plastic beaker of 1.5L, under the powerful stirring of numerical control stirrer, add 200g aluminium nitride powder (α type aluminium nitride/β type aluminium nitride=1/2, size and ratio 0.5 μ m/4.0 μ m=3/1), mix.In the 3L glass beaker, add the 1000g20% silicon sol, stir down slowly adding mixed powder, treat (beaker bottom does not have settling) behind the component homodisperse, press composite phase-change material total amount 0.02 ‰ ratio, slowly drip 1% alum liquor, continue to stir, until whole gelations.The beaker that will contain gel changes in the air dry oven, and freeze-day with constant temperature 36h under 80 ℃ of temperature is cooled to room temperature, and xerogel is taken out, and smashs to pieces in mortar, changes in the beaker again, and powerful mechanical stirring gets powder.
(2) powder is changed in the 2L four-hole boiling flask that is equipped with stirrer, nitrogen tube, return line, dropping funnel; stir following 40 ℃ and vacuumize 3h; oil bath heats to 120 ℃ then; the condensing reflux pipe of fetching boiling water, logical nitrogen protection is in powder gross weight 0.8% ratio; drip silane coupling agent K560; behind the pending 3h, lower the temperature, stop to stir, reflux, lead to nitrogen, obtain the composite phase-change material powder.
(3),, carry out compressing tablet under the pressure 20MPa condition and get block 80 ℃ of temperature with the composite phase-change material powder.
(1) under the room temperature, add 600g polyoxyethylene glycol powder (polyoxyethylene glycol 5000 and cetomacrogol 1000 0 mix by 1/1) in the plastic beaker of 1.5L, under the powerful stirring of numerical control stirrer, add 150g aluminium nitride powder (α type aluminium nitride/β type aluminium nitride=1/1, size and ratio are mixed by 0.5 μ m/4.0 μ m=2/1), mix.In the 3L glass beaker, add the 1250g20% silicon sol, stir down slowly adding mixed powder, treat (beaker bottom does not have settling) behind the component homodisperse, press composite phase-change material total amount 0.03 ‰ ratio, slowly drip 1% liquor alumini chloridi, continue to stir, until whole gelations.The beaker that will contain gel changes in the air dry oven, and freeze-day with constant temperature 48h under 80 ℃ of temperature is cooled to room temperature, and xerogel is taken out, and smashs to pieces in mortar, changes in the beaker again, and powerful mechanical stirring gets powder.
(2) powder is changed in the 2L four-hole boiling flask that is equipped with stirrer, nitrogen tube, return line, dropping funnel; stir following 40 ℃ and vacuumize 3h; oil bath heats to 120 ℃ then; the condensing reflux pipe of fetching boiling water, logical nitrogen protection is in powder gross weight 1.0% ratio; drip silane coupling agent K550; behind the pending 3h, lower the temperature, stop to stir, reflux, lead to nitrogen, obtain composite phase-change material.
(3),, carry out compressing tablet under the pressure 20MPa condition and get block 70 ℃ of temperature with the composite phase-change material powder.
(1) under the room temperature, add 600g polyoxyethylene glycol powder (polyoxyethylene glycol 5000 and cetomacrogol 1000 0 mix by 1/2) in the plastic beaker of 1.5L, powder, under the powerful stirring of numerical control stirrer, add 200g aluminium nitride powder (α type aluminium nitride/β type aluminium nitride=1/2, size and ratio 0.5 μ m/4.0 μ m=2/1), mix.In the 3L glass beaker, add the 1000g20% silicon sol, stir and slowly add mixed powder down, treat the component homodisperse after, press composite phase-change material total amount 0.04 ‰ ratio, slowly drip 1% magnesium chloride solution, continue stirring, until whole gelations.The beaker that will contain gel changes in the air dry oven, and freeze-day with constant temperature 48h under 80 ℃ of temperature is cooled to room temperature, and xerogel is taken out, and smashs to pieces in mortar, changes in the beaker again, and powerful mechanical stirring gets powder.
(2) powder is changed in the 2L four-hole boiling flask that is equipped with stirrer, nitrogen tube, return line, dropping funnel; stir following 40 ℃ and vacuumize 3h; oil bath heats to 120 ℃ then; the condensing reflux pipe of fetching boiling water, logical nitrogen protection is in powder gross weight 1% ratio; drip silane coupling agent K550; behind the pending 3h, lower the temperature, stop to stir, reflux, lead to nitrogen, obtain the composite phase-change material powder.
(3),, carry out compressing tablet under the pressure 15MPa condition and get block 70 ℃ of temperature with the composite phase-change material powder.
Embodiment 4
(1) under the room temperature, add 600g polyoxyethylene glycol powder (Macrogol 3000 and polyethylene glycol 1500 0 mix by 1/2) in the plastic beaker of 1.5L, under the powerful stirring of numerical control stirrer, add 200g aluminium nitride powder (α type aluminium nitride/β type aluminium nitride=1/2, size and ratio 0.5 μ m/4.0 μ m=3/1), mix.In the 3L glass beaker, add the 1250g20% silicon sol, stir down slowly adding mixed powder, treat (beaker bottom does not have settling) behind the component homodisperse, press composite phase-change material total amount 0.03 ‰ ratio, slowly drip 1% aluminum nitrate solution, continue to stir, until whole gelations.The beaker that will contain gel changes in the air dry oven, and freeze-day with constant temperature 48h under 80 ℃ of temperature is cooled to room temperature, and xerogel is taken out, and smashs to pieces in mortar, changes in the beaker again, and powerful mechanical stirring gets powder.
(2) powder is changed in the 2L four-hole boiling flask that is equipped with stirrer, nitrogen tube, return line, dropping funnel; stir following 40 ℃ and vacuumize 3h; oil bath heats to 120 ℃ then; the condensing reflux pipe of fetching boiling water, logical nitrogen protection is in powder gross weight 1.0% ratio; drip silane coupling agent K550; behind the pending 3h, lower the temperature, stop to stir, reflux, lead to nitrogen, obtain the composite phase-change material powder.
(3),, carry out compressing tablet under the pressure 20MPa condition and get block 80 ℃ of temperature with the composite phase-change material powder.
(1) under the room temperature, add 600g polyoxyethylene glycol powder (Macrogol 3000 and cetomacrogol 1000 0 mix by 1/2) in the plastic beaker of 1.5L, under the powerful stirring of numerical control stirrer, add 200g aluminium nitride powder (α type aluminium nitride/β type aluminium nitride=1/2, size and ratio 1.0 μ m/3.0 μ m=3/1), mix.In the 3L glass beaker, add the 1000g20% silicon sol, stir down slowly adding mixed powder, treat (beaker bottom does not have settling) behind the component homodisperse, press composite phase-change material total amount 0.02 ‰ ratio, slowly drip 1% alum liquor, continue to stir, until whole gelations.The beaker that will contain gel changes in the air dry oven, and freeze-day with constant temperature 36h under 80 ℃ of temperature is cooled to room temperature, and xerogel is taken out, and smashs to pieces in mortar, changes in the beaker again, and powerful mechanical stirring gets powder.
(2) powder is changed in the 2L four-hole boiling flask that is equipped with stirrer, nitrogen tube, return line, dropping funnel; stir following 40 ℃ and vacuumize 3h; oil bath heats to 120 ℃ then; the condensing reflux pipe of fetching boiling water, logical nitrogen protection is in powder gross weight 1.0% ratio; drip silane coupling agent K550; behind the pending 3h, lower the temperature, stop to stir, reflux, lead to nitrogen, obtain composite phase-change material powder of the present invention.
(3),, carry out compressing tablet under the pressure 15MPa condition and get block 70 ℃ of temperature with the composite phase-change material powder.
As shown in Figure 1, polyoxyethylene glycol is an organic phase change material, its thermal conductivity low (0.2546W/mK), (polyoxyethylene glycol/SiO after adding the silicon-dioxide setting
2), thermal conductivity slightly improves (0.2985W/mK), and amplification is limited.When adding aluminium nitride, in embodiment 1,2,3, the thermal conductivity of prepared high heat conduction, the inorganic-organic composite phase-change material of setting is respectively 0.7541,0.6531,0.7266W/mK.With pure PEG ratio, amplification is respectively 196.2,156.5,185.4%.
As shown in Figure 2, Fig. 2 (a) is 60 ℃ of polarized light microscopy figure of pure polyoxyethylene glycol down, demonstrates tangible crystalline orientation.The polarized light microscopy figure of Fig. 2 (b) pure polyoxyethylene glycol when being warmed up to 64 ℃, the polyalkylene glycol moiety fusion, near Fig. 2 (c) (68 ℃) when reaching the fusing point, the polarized light microscopy figure of pure polyoxyethylene glycol, polyoxyethylene glycol all dissolve, the generation bubble.Fig. 2 (d) is embodiment 1 prepared high heat conduction and the figuration composite phase-changing material polarized light microscopy figure 60~110 ℃ of range of temperature, and it still keeps not trickling, and shape stability is good.
Fig. 3 is the Electronic Speculum figure of embodiment 1 prepared high heat conduction and figuration composite phase-changing material.As shown in Figure 3, the composite particles size does not produce agglomeration in nanometer range, illustrates that the inorganic-organic composite material each component that adopts colloidal sol-gel process to make is evenly distributed.
Fig. 4 is the DSC curve of polyoxyethylene glycol and embodiment 1 prepared high heat conduction and figuration composite phase-changing material.The polyoxyethylene glycol phase change material has quite high heat storage capacity (187.3J/g), and transformation temperature is 67.18 ℃.After compound, the melting enthalpy of composite phase-change material still higher (108.1J/g), the shared mark of polyoxyethylene glycol (60%) is suitable in its melting enthalpy data (being pure polyoxyethylene glycol 57.7%) and the composite phase-change material, SiO
2, moving into of aluminium nitride be setting and strengthened the thermal conductivity effect; But silicon-dioxide and aluminium nitride add, and cause the polyoxyethylene glycol crystallization to produce defective, thereby the unit latent heat of phase change of composite phase-change material, transformation temperature (66.08 ℃) descend to some extent.
Fig. 5 is the sample thermal conductivity test pattern at different pressures condition lower sheeting of high heat conduction of the present invention and figuration composite phase-changing material, as shown in Figure 5, pressure low (5MPa), the block moulding is poor, possible air packing therein, heat conductivility is poor, along with the increase of pressure, thermal conductivity of composite materials increases, and illustrates that block hollow gas is less still to not having substantially.Behind the pressure that reaches 15MPa, thermal conductivity is tending towards definite value.
Claims (10)
1, the preparation method of a kind of high heat conduction and figuration composite phase-changing material is characterized in that comprising the steps:
(1) aluminium nitride powder and polyoxyethylene glycol powder are mixed, join in the silicon sol, drip promotor, stir, colloidal sol-gel reaction takes place, form the three-dimensional network gel;
(2), smash to pieces and obtain the gel powder with behind the three-dimensional network gel drying;
(3) the gel powder is removed moisture, under nitrogen protection and 120 ℃, adds properties-correcting agent;
The parts by weight of described each component are as follows:
Aluminium nitride 5~30
Silicon sol 20
Polyoxyethylene glycol 40~85
Promotor 0.01~0.1
Properties-correcting agent 0.1~1.5
The polyoxyethylene glycol number-average molecular weight is 1000~20000; Described promotor is a kind of or more than one mixtures in magnesium chloride, calcium chloride, aluminum chloride, the Tai-Ace S 150; Described properties-correcting agent is organo silane coupling agent.
2, method according to claim 1 is characterized in that further comprising the steps of:
(4) material that obtains of step (3) is 60~120 ℃ in temperature, and pressure is that 5~25Mpa compressing tablet makes block.
3, method according to claim 1 and 2 is characterized in that described organo silane coupling agent is aminopropyl triethoxysilane and/or glycidyl ether oxygen propyl trimethoxy silicane.
4, method according to claim 3 is characterized in that the parts by weight of described aluminium nitride, silicon sol, promotor, properties-correcting agent are as follows:
Aluminium nitride 10~20
Silicon sol 20
Promotor 0.01~0.03
Properties-correcting agent 0.5~1.0.
5, method according to claim 4 is characterized in that in the step (1), the consumption of polyoxyethylene glycol for its molecular weight ranges be 3000~6000 with the molecular weight polyethylene glycol scope be 10000~20000 composite by 0.5~1/1.
6, method according to claim 5 is characterized in that in the described step (1), and the particle size range of aluminium nitride powder is that 0.5~5 μ m, crystal formation are α, β type, obtains by the aluminium nitride powder of different-grain diameter, different crystal forms is composite.
7, method according to claim 6 is characterized in that aluminium nitride by α type aluminium nitride/β type aluminium nitride=1/2, and size and weight ratio thereof are respectively by 0.5~1.0/3.0~5.0 μ m, 3/1 composite obtaining.
8, method according to claim 7 is characterized in that in the step (2), and the forced air drying in 80 ℃ of baking ovens of three-dimensional network gel was cooled to room temperature after 24~48 hours, takes out to smash to pieces and to stir to obtain the gel powder.
9, method according to claim 8 is characterized in that in the step (3) the gel powder being vacuumized under 40 ℃ 2~4 hours, removes moisture.
10, the high heat conduction and the figuration composite phase-changing material of the described method preparation of one of claim 1-9.
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JP5102179B2 (en) * | 2008-11-12 | 2012-12-19 | 日東電工株式会社 | Thermally conductive composition and method for producing the same |
CN101824308A (en) * | 2010-05-18 | 2010-09-08 | 陕西科技大学 | Preparation method of composite phase change material and preparation method of leather added with same |
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CN103374333B (en) * | 2012-04-13 | 2016-04-27 | 南京德朔实业有限公司 | Composite phase change material |
CN103420668A (en) * | 2012-05-21 | 2013-12-04 | 天津德仕能科技有限公司 | Heat-storing magnesia brick |
CN110028936B (en) * | 2019-03-19 | 2021-10-08 | 北京工商大学 | Preparation method of cross-linked network-shaped phase-change material |
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