CN104830280B - A kind of shaping phase-change material for passive type Thermal protection and preparation method thereof - Google Patents
A kind of shaping phase-change material for passive type Thermal protection and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of medium temperature composite shape-setting phase-change heat-storage material available for passive type Thermal protection.The composite shape-setting phase-change heat-storage material is using metal nanometer line as heat filling, using sugar alcohol as phase-change heat-storage material.Its preparation method is：Metal nanometer line and sugar alcohol are distributed in absolute ethyl alcohol in the presence of supersound process and surfactant first and form stable suspension, then add aniline and organic acid is well mixed, adding oxidant makes aniline polymerization into polyaniline and is deposited on the surface of sugar alcohol/metal nanometer line particle, and composite shape-setting phase-change heat-storage material is obtained after isolation of purified.Obtained composite shape-setting phase-change heat-storage material by this method, technique is simple, and cost is low；With high latent heat of phase change, heat conductivility is moderate, and without encapsulation, effectively improves the performance of glycitols phase-change heat-storage material, expanded its application.
Description
Technical field
The present invention relates to the preparation of composite shape-setting phase-change heat-storage material, specifically a kind of tool of doping metals nano wire
There is very high latent heat of phase change, and the medium temperature when temperature is below or above its phase transition temperature in solid-state and dimensionally stable is compound fixed
Shape phase-change heat-storage material and preparation method thereof, the heat conductivility of the material is moderate, can be used as the heat accumulation of passive type thermal protection system
Material.
Background technology
Phase-change heat-storage material is that by material phase in version occurs for one kind to absorb or release a large amount of heat energy, material self-temperature
Material that is constant or varying less.The application of phase-change heat-storage material can be divided into two major classes：One kind is storage heat energy to realize energy
The efficient utilization of amount；One kind is passive type Thermal protection, i.e., by absorbing or discharging the heat discharged from environment or protected object body,
A thermal boundary is produced between environment and protected object body and protected object is in suitable temperature environment simultaneously.No
Which field be applied to by by phase-change heat-storage material, its heat storage capacity is all the bigger the better, but the requirement to heat conductivility has
Institute is different.The usable phase-change heat-storage material of storage heat requires that thermal conductivity factor is the higher the better, to realize the quick absorption of heat or release
Put；The phase-change heat-storage material of Thermal protection then requires that thermal conductivity factor is moderate, and can have certain suction exotherm rate, and can rises
To the effect of thermal boundary, so that temperature does not produce excessive fluctuation.
The phase-change heat-storage material of most study is solid-liquid phase change heat accumulating at present, it have larger latent heat of phase change and
Less phase transformation Volume Changes.From material character solid-liquid phase change heat accumulating can be divided into inorganic phase-change heat-storage material and
Organic phase-change heat-storage material.Inorganic phase-change heat-storage material has larger phase-change thermal storage capacity, but severe corrosive be present
With transition kinetics poor-performing, the big and unstable deficiency of degree of supercooling.The advantages of organic phase-change heat-storage material is corrosion-free
Property, transition kinetics performance is good, no supercooling, and stability is very good, and application is more convenient, but its heat conductivility is very poor, leads to
Often only 0.2~0.3W/mK or so, it is necessary to regulate and control to its heat conductivility.Metal nano has that thermal conductivity factor is higher, than
The characteristics of surface area is high, and draw ratio is big, it is a kind of preferably enhanced thermal conduction filler.In view of the heat storage capacity of material, metal is received
Meter Bu Neng additions are excessive, so as to get the thermal conductivity factor of composite phase-change heat-storage material will not be very high, but be in moderate level,
It just can be applied to passive type Thermal protection field.
Another problem existing for solid-liquid phase change heat accumulating is liquid be present during use, it is therefore necessary to solves material
The problem of material encapsulation.One solution is that solid-liquid phase change heat accumulating is changed into fixed phase change heat accumulating.When temperature height
When the transformation temperature of fixed phase change heat accumulating, it is macroscopically still behaving as solid-state, solves the problems, such as encapsulation.In addition,
In fixed phase change heat accumulating, the content of backing material can be very low, therefore has very high latent heat of phase change；The preparation of material
Process is generally straightforward, and this is main advantage of the fixed phase change heat accumulating compared to microcapsule phase-change heat accumulating.Sugar alcohol
As a kind of organic phase-change heat-storage material, its solid-liquid phase change temperature has high class material between 83~190 degree
Latent heat of phase change, it is also a kind of environmentally friendly material, and sweetener has been applied in food additives field.But conduct
Solid-liquid phase change heat accumulating, it must solve the problems, such as encapsulation.Polyaniline is a kind of conducting polymer composite, and preparation process is non-
It is often simple, while it has excellent environmental stability and heat endurance, will not soften before pyrolysis, can be used as a kind of excellent
Backing material be applied to fixed phase change heat accumulating field.In view of its heat endurance, determine when being applied to glycitols
During the backing material of shape phase-change heat-storage material, compared to other high polymer materials, polyaniline has more obvious advantage.
Based on this, the invention discloses one kind using polyaniline as backing material, using sugar alcohol as phase-change heat-storage material, with metal
Nano wire is composite shape-setting phase-change heat-storage material of heat filling and preparation method thereof.The composite shape-setting phase prepared by this method
Change heat storage material, heat filling are anchored by backing material, will not be settled during the use of composite shape-setting phase-change heat-storage material
Separate and influence its performance.Meanwhile the composite shape-setting phase-change heat-storage material heat conductivility obtained is moderate, can be used as relevant temperature
In the range of passive type thermal protection system heat accumulating.
The content of the invention
It is an object of the invention to provide a kind of composite shape-setting phase-change heat-storage material with high latent heat of phase change and its preparation side
Method.The composite shape-setting phase-change heat-storage material is using polyaniline as backing material, using sugar alcohol as phase-change heat-storage material, with metal nanometer line
For heat filling；Its preparation method is simple, and heat conductivility is moderate, can be used as the heat accumulating of passive type thermal protection system.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method for the composite shape-setting phase-change heat-storage material that can be used as passive type thermal protection system heat accumulating, tool
Body is：First by a certain amount of metal nanometer line and absolute ethyl alcohol be mixed and sonicated for obtaining for 20~60 minutes metal nanometer line/
Absolute ethyl alcohol mixed liquor；A certain amount of sugar alcohol, surfactant and a certain amount of absolute ethyl alcohol are added, and by mixture 50~75
Being stirred at reflux at DEG C makes sugar alcohol and surfactant all dissolve；Solution is down to room temperature with vigorous stirring and obtains stable suspersion
Liquid；After aniline and organic acid are added into the suspension and is uniformly mixed, mixture temperature is down to 5~20 DEG C, then
The polymerisation that benzoyl peroxide triggers aniline is added, through filtering, organic solvent washing and drying after reacting 20~30 hours
Obtain composite shape-setting phase-change heat-storage material.
The sugar alcohol be xylitol, D-sorbite, antierythrite, maltitol, mannitol and it is sweet and pure in one kind；It is described
Metal nanometer line is one kind of copper nano-wire and nano silver wire；The surfactant is Macrogol 4000, polyethylene glycol
6000th, one kind in PEG 8000, PEG20000 and PEG 20000；The organic solvent is absolute ethyl alcohol
Or one kind of acetone, the organic acid are one kind of p-methyl benzenesulfonic acid and 5-sulphosalicylic acid.
The dosage of the sugar alcohol is the 70~85% of sugar alcohol and aniline quality sum, sugar in the obtained stable suspension
The content of alcohol is 16.7~25.0 g/L, and the amount of a certain amount of absolute ethyl alcohol of the addition is the metal nanometer line/anhydrous
1~2.33 times of the volume of absolute ethyl alcohol used in alcohol mixeding liquid, the dosage of the nano silver wire is sugar alcohol and aniline used
The 5~67% of quality sum, the content of metal nanometer line is 3~42 g/L in the metal nanometer line/absolute ethyl alcohol mixed liquor,
The dosage of surfactant is the 35~60% of sugar alcohol quality used, the dosage of the organic acid is it is dissolved in suspension
Its concentration is 0.068~0.18mol/L afterwards, and the benzoyl peroxide dosage is the 2~3.5 of the amount of the material of aniline used
Times.
In the composite shape-setting phase-change heat-storage material, polyaniline is backing material, and sugar alcohol is phase-change heat-storage material, and metal is received
Rice noodles are heat filling；When temperature is higher than sugar alcohol fusing point contained by phase-change heat-storage material containing composite shape-setting, the composite shape-setting phase transformation
Heat accumulating outward appearance is in still solid-state and dimensionally stable, and the thermal conductivity factor of composite shape-setting phase-change heat-storage material is with metal nanometer line
The increase of content and increase.
The invention has the advantages that.
The invention provides a kind of composite shape-setting phase-change heat-storage material of doping metals nano wire and preparation method thereof, the material
Material has high latent heat of phase change, and heat conductivility is moderate, can be used as the heat accumulating of passive type thermal protection system.Fid simultaneously
The thermal stability of material polyaniline fully meets the requirement of composite shape-setting phase-change heat-storage material operating temperature.The composite shape-setting phase transformation
The preparation method of heat accumulating is simple, and cost is relatively low.The property of glycitols phase-change heat-storage material can effectively be improved using the present invention
Can, expand its application.
Embodiment
The present invention is described in further detail with reference to specific embodiment, but these embodiments are not intended to limit the present invention
Scope.
The present invention uses Q2000 type differential scanning calorimeters caused by TA companies of the U.S.（DSC）As follows to described
The thermal storage performance of composite shape-setting phase-change heat-storage material is tested：The composite shape-setting phase-change heat-storage material for weighing 1.5~4mg is put into
In sample crucible, before and after the phase transition temperature of phase-change heat-storage material within the temperature range of about 40 DEG C, with 10 DEG C/min heating speed
Rate is scanned；Then the program carried using instrument is handled experimental result, obtains prepared composite shape-setting phase transformation
Starting phase transition temperature, phase transformation peak temperature and the latent heat of phase change of heat accumulating.
The DRX-II-RW types heat conduction coefficient tester that the present invention is produced using Xiang Tan Hua Feng companies determines the composite shape-setting
The thermal conductivity factor of phase-change heat-storage material, detailed process are：1.5g or so composite shape-setting phase-change heat-storage materials are weighed, are existed with tablet press machine
A cylinder is pressed under 1MPa pressure, the temperature of cooling water of the hot-side temperature for setting instrument with flowing through cold end is permanent
Fixed, two temperatures difference is 15 DEG C, and the thermal conductivity factor that software measures material is carried using instrument after the temperature stabilization of hot junction and cold end.
Embodiment 1.
1）Prepare suspension：0.204g nano silver wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 30 minutes nano silver wire/absolute ethyl alcohol mixed liquor；2.0g antierythrites, 0.7g polyethylene glycol are added toward above-mentioned mixed liquor
10000 with 60mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes erythrose and polyethylene glycol is completely dissolved, stop
Only heat, be stirred vigorously, allow system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 1.72g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：2.658 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 116.6 DEG C, phase transformation peak temperature is 121.0 DEG C, phase
Change latent heat is 223.6J/g, thermal conductivity factor 0.349W/mK.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 130 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 2.
1）Prepare suspension：1.67g nano silver wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 60 minutes nano silver wire/absolute ethyl alcohol mixed liquor；2.0g antierythrites, 0.7g polyethylene glycol are added toward above-mentioned mixed liquor
10000 with 60mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes erythrose and polyethylene glycol is completely dissolved, stop
Only heat, be stirred vigorously, allow system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 1.72g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：3.315 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 113.7 DEG C, phase transformation peak temperature is 120.5 DEG C, phase
Change latent heat is 186.8J/g, the W/mK of thermal conductivity factor 0.845.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 130 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 3.
1）Prepare suspension：0.124g nano silver wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 20 minutes nano silver wire/absolute ethyl alcohol mixed liquor；2.0g antierythrites, 1g polyethylene glycol are added toward above-mentioned mixed liquor
10000 with 40mL absolute ethyl alcohols, be put into 70 DEG C of water-bath, after return stirring makes erythrose and polyethylene glycol is completely dissolved, stop
Only heat, be stirred vigorously, allow system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.35 g aniline and 0.94g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration cold bath, it is stirred vigorously and mixture temperature is down to 10~20 DEG C.
3）Aniline polymerization：3.185 g benzoyl peroxides are added into above-mentioned 10~20 DEG C of mixtures and trigger aniline
Polymerisation, and allow mixture to heat up naturally, react 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 112.0 DEG C, phase transformation peak temperature is 120.5 DEG C, phase
Change latent heat is 232.1J/g, thermal conductivity factor 0.297W/mK.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 130 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 4.
1）Prepare suspension：1g nano silver wires are taken, are mixed in 50mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated 40 points
Clock obtains nano silver wire/absolute ethyl alcohol mixed liquor；2.0g antierythrites, 1.2g PEG20000s are added toward above-mentioned mixed liquor
With 70mL absolute ethyl alcohols, be put into 50 DEG C of water-bath, after return stirring makes erythrose and polyethylene glycol is completely dissolved, stop plus
Heat, it is stirred vigorously, allows system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.85 g aniline and 3.7g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After even, then by mixture immigration cold bath, it is stirred vigorously and mixture temperature is down to 10~20 DEG C.
3）Aniline polymerization：4.42 g benzoyl peroxides are added into above-mentioned 10~20 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature be 113.4 DEG C, phase transformation peak temperature be 119.7 DEG C and
Latent heat of phase change is 195.8J/g, the W/mK of thermal conductivity factor 0.694.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 130 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 5.
1）Prepare suspension：0.63g nano silver wires are taken, are mixed in 30mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 30 minutes nano silver wire/absolute ethyl alcohol mixed liquor；2.0g xylitols, 0.9g polyethylene glycol are added toward above-mentioned mixed liquor
20000 with 70mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes xylitol and polyethylene glycol is completely dissolved, stop
Only heat, be stirred vigorously, allow system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 1.72g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：2.658 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 87.8 DEG C, phase transformation peak temperature is 94.1 DEG C, phase transformation
Latent heat is 154.6J/g, thermal conductivity factor 0.563W/mK.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 110 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 6.
1）Prepare suspension：1.08g nano silver wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 30 minutes nano silver wire/absolute ethyl alcohol mixed liquor；2.0g D-sorbites, 1.2g polyethylene glycol are added toward above-mentioned mixed liquor
4000 with 60mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes D-sorbite and polyethylene glycol is completely dissolved, stop
Only heat, be stirred vigorously, allow system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 3.44g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：3.315 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 88.3 DEG C, phase transformation peak temperature is 94.1 DEG C and phase
Change latent heat is 102.6J/g, thermal conductivity factor 0.746W/mK.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 110 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 7.
1）Prepare suspension：1.67g copper nano-wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 30 minutes copper nano-wire/absolute ethyl alcohol mixed liquor；2.0g maltitols, 1g PEG 8000s are added toward above-mentioned mixed liquor
With 60mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes maltitol and polyethylene glycol is completely dissolved, stop plus
Heat, it is stirred vigorously, allows system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 2.542g5- sulfonic groups salicylic acid are added into the suspension and is stirred
After well mixed, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：2.658 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：By after the completion of reaction mixture filter, filter cake is washed with acetone, then by filter cake in
60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 143.6 DEG C, phase transformation peak temperature is 147.9 DEG C, phase
Change latent heat is 86.5J/g, the W/mK of thermal conductivity factor 0.837.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 160 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 8.
1）Prepare suspension：0.63g copper nano-wires are taken, are mixed in 30mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 30 minutes copper nano-wire/absolute ethyl alcohol mixed liquor；2.0g mannitol, 0.9g Macrogol 6000s are added toward above-mentioned mixed liquor
With 70mL absolute ethyl alcohols, be put into 75 DEG C of water-bath, after return stirring makes mannitol and polyethylene glycol is completely dissolved, stop plus
Heat, it is stirred vigorously, allows system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 1.72g p-methyl benzenesulfonic acids are added into the suspension and is stirred
After uniformly, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：2.658 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：Mixture after the completion of reaction is filtered, filter cake is washed with absolute ethyl alcohol, then will filter
Cake is in 60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 161.8 DEG C, phase transformation peak temperature is 165.7 DEG C, phase
Change latent heat is 205.6J/g, the W/mK of thermal conductivity factor 0.578.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 190 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Embodiment 9.
1）Prepare suspension：0.28g copper nano-wires are taken, are mixed in 40mL absolute ethyl alcohols in round-bottomed flask, are ultrasonically treated
Obtain within 20 minutes copper nano-wire/absolute ethyl alcohol mixed liquor；Sweet and pure, the 0.9g PEG20000s toward above-mentioned mixed liquor addition 2.0g
With 60mL absolute ethyl alcohols, it is put into 75 DEG C of water-bath, after return stirring is completely dissolved sweet and pure and polyethylene glycol, stops heating,
It is stirred vigorously, allows system to cool to greenhouse and obtain stable suspension.
2）Suspension cools：0.51 g aniline and 2.03g 5- sulfonic groups salicylic acids are added into the suspension and is stirred
After well mixed, then by mixture immigration ice-water bath, it is stirred vigorously and mixture temperature is down to 5~10 DEG C.
3）Aniline polymerization：3.978 g benzoyl peroxides are added into above-mentioned 5~10 DEG C of mixtures and trigger the poly- of aniline
Reaction is closed, and allows mixture to heat up naturally, is reacted 24 hours.
4）Isolate and purify product：Mixture after the completion of reaction is filtered, filter cake is washed with absolute ethyl alcohol, then will filter
Cake is in 60 DEG C of drying composite shape-setting phase-change heat-storage materials.
5）Heat accumulation and thermal conductivity test result：Starting phase transition temperature is 181.4 DEG C, phase transformation peak temperature is 187.5 DEG C, phase
Change latent heat is 214.8J/g, the W/mK of thermal conductivity factor 0.429.
6）Stability test：Material is pressed into a cylinder with tablet press machine under 1MPa pressure, is put into 200 DEG C
Insulating box, cylindrical shape is observed after 12 hours and does not change and is converged without liquid and is leaked.
Claims (2)
1. a kind of preparation method of composite shape-setting phase-change heat-storage material, it is characterised in that detailed process is：First by a certain amount of gold
Category nano wire is mixed and sonicated for obtaining within 20~60 minutes metal nanometer line/absolute ethyl alcohol mixed liquor with absolute ethyl alcohol；Again plus
Enter a certain amount of sugar alcohol, surfactant and a certain amount of absolute ethyl alcohol, and mixture is stirred at reflux at 50~75 DEG C makes sugar alcohol
All dissolved with surfactant；Solution is down to room temperature with vigorous stirring and obtains suspension；Benzene is added into the suspension
Amine and organic acid and after being uniformly mixed, are down to 5~20 DEG C by mixture temperature, then add benzoyl peroxide and trigger benzene
The polymerisation of amine, after reaction 20~30 hours through filtering, organic solvent washing and be dried to obtain composite shape-setting phase-change thermal storage material
Material；The sugar alcohol be xylitol, D-sorbite, antierythrite, maltitol, mannitol and it is sweet and pure in one kind, the metal
Nano wire is one kind of copper nano-wire and nano silver wire, and the surfactant is Macrogol 4000, Macrogol 6000, gathered
One kind in ethylene glycol 8000, PEG20000 and PEG 20000, it is used organic during the organic solvent washing
Solvent is one kind of absolute ethyl alcohol or acetone, and the organic acid is one kind of p-methyl benzenesulfonic acid and 5-sulphosalicylic acid；It is described
The dosage of sugar alcohol is the 70~85% of sugar alcohol and aniline quality sum, in the obtained suspension content of sugar alcohol for 16.7~
25.0 g/L, the amount of a certain amount of absolute ethyl alcohol of the addition is used in the metal nanometer line/absolute ethyl alcohol mixed liquor
1~2.33 times of the volume of absolute ethyl alcohol, the dosage of the metal nanometer line is sugar alcohol used with the 5 of aniline quality sum~
67%, the content of metal nanometer line is 3~42 g/L in the metal nanometer line/absolute ethyl alcohol mixed liquor, the surfactant
Dosage is the 35~60% of sugar alcohol quality used, the dosage of the organic acid be make its be dissolved in suspension after its concentration be 0.068
~0.18mol/L, the benzoyl peroxide dosage are 2~3.5 times of the amount of the material of aniline used.
2. according to the preparation method of the composite shape-setting phase-change heat-storage material described in claim 1, it is characterised in that prepared to obtain
Composite shape-setting phase-change heat-storage material in, polyaniline is backing material, and sugar alcohol is phase-change heat-storage material, and metal nanometer line is heat conduction
Filler；When temperature is higher than sugar alcohol fusing point contained by composite shape-setting phase-change heat-storage material, the composite shape-setting phase-change heat-storage material outward appearance
Still it is in solid-state and dimensionally stable；The composite shape-setting phase-change heat-storage material heat conductivility is moderate, can be used as passive type thermal protection system
Heat accumulating.
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| CN107446554B (en) * | 2017-09-22 | 2020-09-18 | 浙江海洋大学 | Preparation method of wide phase-change temperature zone shape-stabilized phase-change material |
| CN109370538B (en) * | 2018-11-26 | 2020-05-22 | 浙江大学 | Phase change coolant for refreshing pleurotus eryngii and preparation method thereof |
| CN114539980A (en) * | 2020-11-27 | 2022-05-27 | 中国科学院大连化学物理研究所 | Phase-change material capable of storing energy at room temperature for long time and preparation and application thereof |
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