CN107446554A - A kind of preparation method of wide transition temperature area shaping phase-change material - Google Patents
A kind of preparation method of wide transition temperature area shaping phase-change material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of wide transition temperature area shaping phase-change material, the preparation method comprises the following steps：The preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide；Shaping phase-change material laurate/copper/silver/SBA 15 preparation；Shaping phase-change material polyethylene glycol/copper/silver/SBA 15 preparation；Shaping phase-change material stearic acid/copper/silver/SBA 15 preparation；The preparation of wide transition temperature area shaping phase-change material；The preparation of wide transition temperature area shaping phase-change material.Material of the present invention effectively avoids caused by directly mixing that core reacts to each other, amalgamation is poor, enthalpy of phase change is low, cost is cheap, and improves its heat conductivility.
Description
Technical field
The invention belongs to phase-change material field, and in particular to a kind of preparation method of wide transition temperature area shaping phase-change material.
Background technology
The energy is the technology that the mankind depend on for existence and development, but is usually present time and spatially between energy supply
Unmatched contradiction, current many energy can not obtain rationally sufficiently utilizing.
In energy storage and application field, phase-change material because with energy storage density it is big, it is repeatable utilize, that stability is good etc. is excellent
Point is widely used in building energy conservation, intelligent thermoregulating fabric, solar energy hot systems, electronic device by more and more concerns
The fields such as radiating, industrial exhaust heat utilization and air-conditioning system.Currently the research to organic shaping phase-change material is concentrated mainly on single
Core, the transition temperature area of the organic shaping phase-change material of pure component is narrower, is mainly used in temperature control packaging, battery thermal management, electronics member
Device temperature control etc. has the heat control system of strict demand to temperature.However, in building energy conservation, heliogreenhouse, Intelligent heat storage clothes etc.
Field, phase-changing energy storage material suction/thermal discharge are had a great influence by season and Changes in weather, cause phase-change material utilization rate and heat accumulation
Amount reduces, and can not give full play to the advantage of its energy storage and energy-conservation.
To strengthen the environmental suitability of phase-change material, its utilization rate and quantity of heat storage are improved, using different organic phase-change materials
Core shaping phase-change material is prepared after material mixing, improves its transition temperature area, but existing core shaping phase-change material is not mainly by
Directly it is mixed with to obtain with phase-change material core, there is that core reacts to each other, amalgamation is poor, enthalpy of phase change is low, heat conductivility is poor
The problems such as.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of wide transition temperature area shaping phase-change material to prepare
Method, the material effectively avoid directly mixing caused by core reacts to each other, amalgamation is poor, enthalpy of phase change is low, cost is cheap, and
Improve its heat conductivility.
To solve prior art problem, the technical scheme that the present invention takes is：
A kind of preparation method of wide transition temperature area shaping phase-change material, comprises the following steps：
Step 1, the preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide
4.0g P123 (PEO-PPOX-PEO triblock copolymer) are added in beaker,
30g distilled water and 120g 1.8-2.2M hydrochloric acid are added, beaker is placed in water-bath, stirs 3h, then adds 8.5g TEOS
(tetraethyl orthosilicate), 35 DEG C stirring 20h, emulsion is transferred in hydrothermal reaction kettle after the completion of reaction, experience crystallization, centrifugation,
Washing, after drying, calcine to obtain mesoporous silicon oxide SBA-15；
Step 2, shaping phase-change material laurate/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, 30mg SBA-15 add 70ml 1g/L laurate (LA)
In ethanol solution, mixture is stirred into 4h at 65 DEG C, dries 24h at a temperature of 80 DEG C afterwards, obtains phase transition temperature as 39
DEG C laurate/copper/silver/SBA-15；
Step 3, shaping phase-change material polyethylene glycol/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, 30mg SBA-15 add 70ml 1g/L polyethylene glycol
In ethanol solution, mixture is stirred into 4h at 65 DEG C, dries 24h at a temperature of 80 DEG C afterwards, obtains phase transition temperature as 50
DEG C PEG/Cu/Ag/SBA-15；
Step 4, shaping phase-change material stearic acid/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, 30mg SBA-15 add the stearic ethanol solutions of 70ml
In, stir 4h at 65 DEG C, then 24h is dried at a temperature of 80 DEG C, obtain preparing stearic acid/copper/silver that phase transition temperature is 60 DEG C/
SBA-15；
Step 5, the preparation of wide transition temperature area shaping phase-change material
By shaping phase-change material laurate/copper/silver/SiO of different phase transition temperatures2, polyethylene glycol/copper/silver/SiO2With it is hard
Resin acid/copper/silver/SiO2It is sufficiently mixed, prepares the wide transition temperature area shaping phase-change material that transition temperature area is 39-60 DEG C.
It is that crystallization temperature is 100 DEG C in step 1, and calcining heat is 500 DEG C, and the molar concentration of hydrochloric acid is as improved
2M。
It is that the molecular weight of polyethylene glycol is 2000 in step 3 as improved.
It is that the concentration of stearic ethanol solution is 1g/L in step 4 as improved.
It is that step 2, the copper nano-wire dosage in step 3 and step 4 is 5mg, and silver nano-grain adds as improved
Measure as 5mg.
It is laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and tristearin in step 5 as improved
The mass ratio of acid/copper/tri- kinds of shaping phase-change materials of silver/SBA-15 is (1-2):(1-2):(1-2).
Principle：The present invention is first with mesopore silicon oxide (SiO2) laurate (LA) preparation phase transition temperature is fixed as 39 DEG C
Laurate/copper/silver/SBA-15 shaping phase-change materials, then mesopore silicon oxide (SiO2) fix polyethylene glycol (PEG) preparation phase transformation
Temperature is 50 DEG C of polyethylene glycol/copper/silver/SBA-15 shaping phase-change materials, recycles mesopore silicon oxide (SiO2) fixed stearic
Sour (CA) prepares stearic acid/copper/silver/SBA-1 shaping phase-change materials that phase transition temperature is 60 DEG C, finally by different phase transition temperatures
Shaping phase-change material laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and stearic acid/copper/silver/SBA-1 press one
Certainty ratio mixes, and prepares the wide transition temperature area shaping phase-change material that transition temperature area is 39 DEG C to 60 DEG C.In addition, add copper nanometer
The heat conductivility of line and the adjustable pitch width transition temperature area shaping phase-change material of silver nano-grain, that has expanded material uses field.
Compared with prior art, advantage of the invention is as follows：
1st, by the way that the phase-change material core of different phase transition temperatures is fixed in mesopore silicon oxide, different phase alternating temperatures are prepared
The shaping phase-change material heat accumulation particle of degree, then the different heat accumulation particle of phase transition temperature is mixed, prepare wide transition temperature area setting
Phase-change material, effectively avoids caused by the directly mixing of phase-change material core that core, which reacts to each other, amalgamation is poor, enthalpy of phase change is low etc. asks
Topic；
2nd, by changing the ratio of different core shaping phase-change materials, and the cooperation of copper nano-wire and silver nano-grain,
The regulation and control of core shaping phase-change material transition temperature area and heat conductivility are realized, expand its application.
Embodiment
The present invention is further described in detail below by specific embodiment.
P123 is the abbreviation of chemical reagent PEO-PPOX-PEO triblock copolymer, purchase
In Sigma-Aldrich (Shanghai) trade Co., Ltd；
TEOS is tetraethyl orthosilicate, is bought in Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1
A kind of preparation method of wide transition temperature area shaping phase-change material, comprises the following steps：
Step 1, the preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide
4.0g P123 are added in beaker, 30g distilled water and 120g 1.8M hydrochloric acid is added, beaker is placed in water-bath
In, 3h is stirred, 8.5g TEOS is then added, 35 DEG C of stirring 20h, emulsion is transferred in hydrothermal reaction kettle after the completion of reaction,
After undergoing crystallization, centrifugation, washing, drying, mesoporous silicon oxide SBA-15 is calcined to obtain；
Step 2, shaping phase-change material laurate/copper/silver/SBA-15 preparation
By 3mg copper nano-wires, 4mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L LA ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 39 DEG C laurate/copper/
Silver/SBA-15；
Step 3, shaping phase-change material polyethylene glycol/copper/silver/SBA-15 preparation
By 3mg copper nano-wires, 4mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L PEG ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 50 DEG C polyethylene glycol/
Copper/silver/SBA-15；
Step 4, shaping phase-change material stearic acid/copper/silver/SBA-15 preparation
By 3mg copper nano-wires, 4mg silver nano-grains, 30mg SBA-15 are added in 70ml Ca ethanol solutions, are stirred at 65 DEG C
4h is mixed, then 24h is dried at a temperature of 80 DEG C, obtains preparing stearic acid/copper/silver/SBA-15 that phase transition temperature is 60 DEG C；
Step 5, the preparation of wide transition temperature area shaping phase-change material
By shaping phase-change material laurate/copper/silver/SBA-15, the polyethylene glycol/copper/silver/SBA-15 of different phase transition temperatures
It is sufficiently mixed with stearic acid/copper/silver/SBA-15, prepares the wide transition temperature area fixed phase change material that transition temperature area is 39-60 DEG C
Material；
Wherein, crystallization temperature is 100 DEG C in step 1, and calcining heat is 500 DEG C.
PEG molecular weight is 2000 in step 3.
The concentration of stearic ethanol solution is 1g/L in step 4.
Laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and stearic acid/copper/silver/SBA-15 in step 5
The mass ratio of three kinds of shaping phase-change materials is 1:1:1.
Embodiment 2
A kind of preparation method of wide transition temperature area shaping phase-change material, comprises the following steps：
Step 1, the preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide
4.0g P123 are added in beaker, 30g distilled water and 120g 2.0M hydrochloric acid is added, beaker is placed in water-bath
In, 3h is stirred, 8.5g TEOS is then added, 35 DEG C of stirring 20h, emulsion is transferred in hydrothermal reaction kettle after the completion of reaction,
After undergoing crystallization, centrifugation, washing, drying, mesoporous silicon oxide SBA-15 is calcined to obtain；
Step 2, shaping phase-change material laurate/copper/silver/SBA-15 preparation
By 5mg copper nano-wires, 5mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L LA ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 39 DEG C laurate/copper/
Silver/SBA-15；
Step 3, shaping phase-change material polyethylene glycol/copper/silver/SBA-15 preparation
By 5mg copper nano-wires, 5mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L PEG ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 50 DEG C polyethylene glycol/
Copper/silver/SBA-15；
Step 4, shaping phase-change material stearic acid/copper/silver/SBA-15 preparation
By 5mg copper nano-wires, 5mg silver nano-grains, 30mg SBA-15 are added in 70ml CA ethanol solutions, are stirred at 65 DEG C
4h is mixed, then 24h is dried at a temperature of 80 DEG C, obtains preparing stearic acid/copper/silver/SBA-15 that phase transition temperature is 60 DEG C；
Step 5, the preparation of wide transition temperature area shaping phase-change material
By shaping phase-change material laurate/copper/silver/SBA-15, the polyethylene glycol/copper/silver/SBA-15 of different phase transition temperatures
It is sufficiently mixed with stearic acid/copper/silver/SBA-15, prepares the wide transition temperature area fixed phase change material that transition temperature area is 39-60 DEG C
Material；
Wherein, crystallization temperature is 100 DEG C in step 1, and calcining heat is 500 DEG C, and the molar concentration of hydrochloric acid is 2M.
PEG molecular weight is 2000 in step 3.
The concentration of stearic ethanol solution is 1g/L in step 4.
Laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and stearic acid/copper/silver/SBA-15 in step 5
The mass ratio of three kinds of shaping phase-change materials is 1:1:1.
Embodiment 3
A kind of preparation method of wide transition temperature area shaping phase-change material, comprises the following steps：
Step 1, the preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide
4.0g P123 are added in beaker, 30g distilled water and 120g 2.2M hydrochloric acid is added, beaker is placed in water-bath
In, 3h is stirred, 8.5g TEOS is then added, 35 DEG C of stirring 20h, emulsion is transferred in hydrothermal reaction kettle after the completion of reaction,
After undergoing crystallization, centrifugation, washing, drying, mesoporous silicon oxide SBA-15 is calcined to obtain；
Step 2, shaping phase-change material laurate/copper/silver/SBA-15 preparation
By 8mg copper nano-wires, 6mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L LA ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 39 DEG C laurate/copper/
Silver/SBA-15；
Step 3, shaping phase-change material polyethylene glycol/copper/silver/SBA-15 preparation
By 8mg copper nano-wires, 6mg silver nano-grains, 30mg SBA-15 are added in 70ml 1g/L PEG ethanol solutions, will
Mixture stirs 4h at 65 DEG C, afterwards at a temperature of 80 DEG C dry 24h, obtain phase transition temperature be 50 DEG C polyethylene glycol/
Copper/silver/SBA-15；
Step 4, shaping phase-change material stearic acid/copper/silver/SBA-15 preparation
By 8mg copper nano-wires, 6mg silver nano-grains, 30mg SBA-15 are added in 70ml CA ethanol solutions, are stirred at 65 DEG C
4h is mixed, then 24h is dried at a temperature of 80 DEG C, obtains preparing stearic acid/copper/silver/SBA-15 that phase transition temperature is 60 DEG C；
Step 5, the preparation of wide transition temperature area shaping phase-change material
By shaping phase-change material laurate/copper/silver/SBA-15, the polyethylene glycol/copper/silver/SBA-15 of different phase transition temperatures
It is sufficiently mixed with stearic acid/copper/silver/SBA-15, prepares the wide transition temperature area fixed phase change material that transition temperature area is 39-60 DEG C
Material；
Wherein, crystallization temperature is 100 DEG C in step 1, and calcining heat is 500 DEG C.
PEG molecular weight is 2000 in step 3.
The concentration of stearic ethanol solution is 1g/L in step 4.
Laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and stearic acid/copper/silver/SBA-15 in step 5
The mass ratio of three kinds of shaping phase-change materials is 1:1:1.
Comparative example 1
In addition to without copper nano-wire, remaining is the same as embodiment 2.
Comparative example 2
In addition to without nano silver wire, remaining is the same as embodiment 2.
Performance detection is carried out to embodiment 1-3 and comparative example 1-2 wide transition temperature area shaping phase-change material, the data obtained is such as
Following table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| Thermal conductivity factor (W (m K)-1) | 0.488 | 0.539 | 0.625 | 0.317 | 0.218 |
It is shown.
It is seen from the above data that the wide transition temperature area shaping phase-change material heat conductivility of the present invention is more preferable, production has been widened
The application field of product.
In addition, the invention is not restricted to above-mentioned embodiment, as long as in without departing from the scope of the present invention, can take various
Mode implements the present invention.
Claims (6)
1. a kind of preparation method of wide transition temperature area shaping phase-change material, it is characterised in that comprise the following steps：
Step 1, the preparation of wide transition temperature area shaping phase-change material carrier mesopore silicon oxide
4.0g P123 are added in beaker, 30g distilled water and 120g 1.8-2.2M hydrochloric acid is added, beaker is placed in water-bath
In, 3h is stirred, 8.5g TEOS is then added, 35 DEG C of stirring 20h, emulsion is transferred in hydrothermal reaction kettle after the completion of reaction,
After undergoing crystallization, centrifugation, washing, drying, mesoporous silicon oxide SBA-15 is calcined to obtain；
Step 2, shaping phase-change material laurate/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, it is molten that 30mg SBA-15 add the lauric ethanol of 70ml 1g/L
In liquid, mixture is stirred into 4h at 65 DEG C, dries 24h at a temperature of 80 DEG C afterwards, obtains the moon that phase transition temperature is 39 DEG C
Cinnamic acid/copper/silver/SBA-15；
Step 3, shaping phase-change material polyethylene glycol/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, 30mg SBA-15 add the ethanol of 70ml 1g/L polyethylene glycol
In solution, mixture is stirred into 4h at 65 DEG C, dries 24h at a temperature of 80 DEG C afterwards, it is 50 DEG C to obtain phase transition temperature
Polyethylene glycol/copper/silver/SBA-15；
Step 4, shaping phase-change material stearic acid/copper/silver/SBA-15 preparation
By 1-10mg copper nano-wires, 1-10mg silver nano-grains, 30mg SBA-15 are added in the stearic ethanol solutions of 70ml,
Stir 4h at 65 DEG C, then 24h dried at a temperature of 80 DEG C, obtain preparing stearic acid/copper/silver that phase transition temperature is 60 DEG C/
SBA-15；
Step 5, the preparation of wide transition temperature area shaping phase-change material
By shaping phase-change material laurate/copper/silver/SiO of different phase transition temperatures2, polyethylene glycol/copper/silver/SiO2With stearic acid/
Copper/silver/SiO2It is sufficiently mixed, prepares the wide transition temperature area shaping phase-change material that transition temperature area is 39-60 DEG C.
2. the preparation method of wide transition temperature area shaping phase-change material according to claim 1, it is characterised in that in step 1
Crystallization temperature is 100 DEG C, and calcining heat is 500 DEG C, and the molar concentration of hydrochloric acid is 2M.
3. the preparation method of wide transition temperature area shaping phase-change material according to claim 1, it is characterised in that in step 3
The molecular weight of polyethylene glycol is 2000.
4. the preparation method of wide transition temperature area shaping phase-change material according to claim 1, it is characterised in that in step 4
Stearic ethanol solution concentration is 1g/L.
5. the preparation method of wide transition temperature area shaping phase-change material according to claim 1, it is characterised in that step 2, step
Rapid 3 and step 4 in the addition of copper nano-wire be 5mg, the addition of nano silver wire is 5mg.
6. the preparation method of wide transition temperature area shaping phase-change material according to claim 1, it is characterised in that in step 5
Laurate/copper/silver/SBA-15, polyethylene glycol/copper/silver/SBA-15 and stearic acid/copper/tri- kinds of silver/SBA-15 fixed phase change materials
The mass ratio of material is (1-2):(1-2):(1-2).
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