CN102786817A - Silica-supported organic alkane phase change material, and preparation method and application thereof - Google Patents
Silica-supported organic alkane phase change material, and preparation method and application thereof Download PDFInfo
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- CN102786817A CN102786817A CN2012102612018A CN201210261201A CN102786817A CN 102786817 A CN102786817 A CN 102786817A CN 2012102612018 A CN2012102612018 A CN 2012102612018A CN 201210261201 A CN201210261201 A CN 201210261201A CN 102786817 A CN102786817 A CN 102786817A
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Abstract
The invention discloses a silica-supported organic alkane phase change material, and a preparation method and application thereof. The material uses hollow mesoporous or multistage porous silica particles with a particle size of 10 to 800 nm and porosity of 30 to 80% as a carrier, then C10-C16 alkanes with a mass accounting for 10% to 13% of the silica particles are loaded on the carrier. The preparation method comprises the following steps: preparing the silica particles from ethyl orthosilicate, hexadecyltrimethoxyammonium bromide and ammonia water in an aqueous ethanol solution or an aqueous ethanol-ether solution; modifying the silica particles with dodecafluoroheptyl-propyl-trimethoxysiloxane; allowing the modified silica particles and the C10-C16 alkanes to undergo adsorption under vacuum so as to obtain the silica-supported organic alkane phase change material; and compounding the phase change material and a resin to obtain an icing preventing coating material. The advantages of the invention are as follows: the phase change material has a long using period, a long term anti-icing effect is good, and the preparation method is simple and costs little.
Description
Technical field
The present invention relates to a kind of silicon dioxide carried organic alkane phase change material and preparation method and application, belong to inoganic particle modified technical field.
Background technology
Phase change material is a kind of chemical material that utilizes latent heat of phase change to come energy storage and exoergic, phase change material when taking place to change mutually, solid through solid-liquid or solid-phase transition process, in less TR, discharge or store great amount of heat.
Organic alkane is one type of important phase change material, and its good stability, latent heat of phase change are high, transformation temperature is adjustable, are with a wide range of applications.The micro encapsulation of organic alkane can be realized solid powdering (Zhou Jianwei, the Yu Dongmei of liquid alkane; Zhao Yunhui, Su Junfeng, Yuan Xiaoyan. organic alkane phase change material and micro encapsulation thereof. chemical progress; 2011,23:695-703), be used for aspects such as heat transfer, temperature control and energy storage more.In addition, organic alkane phase change material also can directly be compound in the material matrix, and has anti-icing performance (Guan Li; Zhang Hui, Yang Yanlian, Wang Chen; Zhang Zhong, Chen Yunfa. a kind of have an anti-icing materials with function. and 2011, CN102241886A).
Utilize the sol-gel ratio juris, with the mesoporous or multistage hole silicon dioxide granule of hollow of emulsion method preparation, median size is about 500nm; Mesoporous aperture is 1 ~ 5nm, and porosity is about 80%, helps micromolecular absorption and migration (Zhao Yunhui; Liu's Zhe, Yuan Xiaoyan, Zhou Jianwei; Li Hui, Yu Dongmei. a kind of have slow-release function super-hydrophobic ice-covering-proof coating and preparation method thereof. and 2012, CN102382536A).Silica particle surface residual hydroxyl and unsaturated link(age), surface energy is higher.Select suitable coupling agent to carry out surface-treated, help absorption organic alkane phase change material.According to the regulation and control of the composite and transformation temperature of organic alkane, load the silicon dioxide granule of phase change material can have the potential application prospect in a plurality of fields.
Silicon dioxide granule and matrix resin through surface-treated have consistency preferably; Simultaneously, utilize the organic alkane phase change material of the mesoporous or multistage hole silicon dioxide granule of hollow load, also help the uniform distribution of phase change material in resin matrix.
Summary of the invention
The objective of the invention is to provide a kind of silicon dioxide carried organic alkane phase change material and preparation method and application.Silicon dioxide carried organic alkane phase change material life cycle is longer, and with resin compounded after, the hydrophobic anti-icing performance of coating is more excellent.The preparation method of this silicon dioxide carried organic alkane phase change material is simple, lower, the easy handling of cost, and can be widely used in a plurality of fields.
The present invention realizes through following technical scheme; A kind of silicon dioxide carried organic alkane phase change material; It is characterized in that, this phase change material be with particle diameter be 10 ~ 800nm, to have porosity be that 30 ~ 80% hollow silicon dioxide granule mesoporous or multistage hole is a carrier, load C
10~ C
16Organic alkane, organic alkane of its load is 10% ~ 13% of silicon-dioxide quality.
The preparation method of silicon dioxide carried organic alkane phase change material of said structure is characterized in that may further comprise the steps:
1) preparation of silicon dioxide granule
Method one: in volumetric concentration was 20 ~ 60% aqueous ethanolic solution, temperature was that 25wt% ammoniacal liquor volume ratio is (0.5 ~ 1.5) by tetraethoxy (TEOS) with concentration: 1 at 10 ~ 30 ℃; Cationic emulsifier hexadecyl trimethoxy brometo de amonio (CTAB) is 1 with tetraethoxy (TEOS) mass ratio: (5 ~ 15); At first in aqueous ethanolic solution, add cationic emulsifier hexadecyl trimethoxy brometo de amonio (CTAB), stirring velocity is under 500 ~ 1000rpm, drips tetraethoxy (TEOS); Emulsification 5 ~ 15mim; Adding concentration then is 25wt% ammoniacal liquor, and reaction 1 ~ 5h is dried 12 ~ 24h down through the throw out that spinning obtains for 60 ~ 80 ℃ in temperature; Be elevated to 300 ~ 600 ℃ of calcining 3 ~ 6h down then in the 20min, obtain hollow mesoporous silicon oxide particle.
Method two: in the mixing solutions of ether, ethanol, deionized water volume ratio 1:2:7, temperature is that 25wt% ammoniacal liquor volume ratio is (3 ~ 7) by tetraethoxy (TEOS) with concentration: 1 at 10 ~ 30 ℃; Cationic emulsifier hexadecyl trimethoxy brometo de amonio (CTAB) is 1 with tetraethoxy (TEOS) mass ratio: (1 ~ 5); At first in mixing solutions, add emulsifying agent CTAB, stirring velocity is under 500 ~ 1000rpm, drips TEOS; Emulsification 5 ~ 15mim; Adding concentration then is 25wt% ammoniacal liquor, and reaction 1 ~ 5h is dried 12 ~ 24h down through the throw out that spinning obtains for 60 ~ 80 ℃ in temperature; Be elevated to 300 ~ 600 ℃ of calcining 3 ~ 6h down then in the 20min, obtain multistage hole silicon dioxide granule.
2) modification of the silicon dioxide granule that makes of step 1)
Mol ratio by the coupling agent of silicon dioxide granule and ten difluoro heptyl propyl trimethoxy siloxanes is 3:1; Be dispersed in silicon dioxide granule in the toluene solution that contains ten difluoro heptyl propyl trimethoxy siloxanes with the cell pulverization machine; Atmospheric pressure reflux reaction 5 ~ 10h under 50 ~ 100 ℃ of temperature; Collect phegma; Till removing totally with toluene wash is also centrifugal to ten difluoro heptyl propyl trimethoxy siloxanes,, obtain the mesoporous or multistage hole silicon dioxide granule of silane coupler modified hollow at 50 ~ 90 ℃ of down dry 12 ~ 24h of temperature.
3) silicon dioxide carried organic alkane phase change material
Silicon dioxide granule and organic alkane C of 2 modifications that make set by step
10~ C
16Mass ratio be (0.02 ~ 0.2): 1; The improved silica particle is added in organic alkane, is under 0.01MPa ~ 0.1MPa in vacuum tightness, and continuously stirring is adsorbed organic alkane phase change material 1 ~ 10h; Whip attachment 10 ~ 20h under normal pressure then; Use toluene wash, spinning again, remove the organic alkane that is adsorbed on silica particle surface, obtain silicon dioxide carried organic alkane phase change material.
The application of silicon dioxide carried organic alkane phase change material of above-mentioned preparation: this silicon dioxide carried organic alkane phase change material and silicone resin are compound, are applied to anti-icing coated material.
Silicon dioxide carried organic alkane phase change material is owing to mesoporous slowly the move to surface of organic alkane from silica particle surface; During with resin compounded; Silicon dioxide carried organic alkane phase change material life cycle is longer; Simultaneously, organic alkane discharges certain latent heat when low temperature, and resin coating has effectively reached the effect of long-term anti-icing.The preparation process of this silicon dioxide carried organic alkane phase change material is simple, and cost is lower.The coated material that prepared phase change material and resin compounded obtain is widely used in the anti-icing field of industries such as aerospace and communication.
Description of drawings
Fig. 1 is the prepared hollow mesoporous silicon oxide of the embodiment of the invention one a step 1 particle TEM photo.
Fig. 2 is the prepared multistage hole silicon dioxide granule TEM photos of the embodiment of the invention two step 1.
Embodiment
Below through specific examples the present invention is described, but the present invention is not only limited to these instances.
Embodiment one
60mL ethanol, 100mL deionized water and 0.3g CTAB are joined in the there-necked flask of 250mL, mix until dissolving, under the 700rpm stirring velocity 25 ℃ of following mechanical stirring; 2mLTEOS is added drop-wise in the above-mentioned mixing solutions, emulsification 10min, adding 2mL concentration is the ammoniacal liquor of 25wt%; Reaction 3h; The throw out that spinning obtains is dried 24h down at 80 ℃, is elevated to 550 ℃ of calcining 5h down then in the 20min, obtains hollow mesoporous silicon oxide particle.
The particle diameter of prepared hollow mesoporous silicon oxide particle is that 500nm, mesoporous size mainly are distributed in 1.5nm and 3nm, porosity are about 80%.
Take by weighing 0.2g hollow mesoporous silicon oxide particle; Be dispersed in the 40mL toluene solution that contains 0.377mL ten difluoro heptyl propyl trimethoxy siloxanes with ultrasonic cell disruptor; Under 80 ℃, back flow reaction 8h, with toluene wash and centrifugal to ten difluoro heptyl propyl trimethoxy siloxanes remove clean till; The throw out that obtains is dry 24h under 80 ℃, obtains the hollow mesoporous silicon oxide particle of modification.
Take by weighing 0.2g and be dispersed in 1.8gC through the hollow mesoporous silicon oxide particle of modification
12Alkane and 4.2gC
14In the mixture of alkane, be under the 0.09MPa in vacuum tightness, continuously stirring is adsorbed organic alkane phase change material 4h; Whip attachment 12h under normal pressure then; Stop absorption, centrifugal twice with toluene wash, obtain the organic alkane phase change material of hollow mesoporous silicon oxide particle load.
Measure charge capacity with anti-STA 449 C that speed of Germany, recording the machine alkane charge capacity that loads in the hollow mesoporous silicon oxide is 12.6% of silicon-dioxide quality.
The hollow mesoporous silicon oxide particle of the organic alkane phase change material of 0.12g load is dispersed in the 2g toluene with ultrasonic cell pulverization machine; The silicone resin uniform mixing that is heating and curing with 2g then; Be coated on 3cm * 3cm aluminium sheet, solidify 30min down at 30 ℃, 75 ℃ solidify 45min down; Solidify 2h down at 150 ℃ again, obtain the anti-icing coating of the organic alkane phase change material of load hollow mesoporous silicon oxide particle.
Embodiment two:
20mL ethanol, 40mL ether, 140mL deionized water and 1gCTAB are joined in the there-necked flask of 250mL, mix until dissolving, under the 700rpm stirring velocity 25 ℃ of following mechanical stirring; 5mLTEOS is added drop-wise in the above-mentioned mixing solutions, emulsification 10min, adding 1.6mL concentration is the ammoniacal liquor of 25wt%; Reaction 4h; The throw out that spinning obtains is dried 24h down at 80 ℃, is elevated to 550 ℃ of calcining 5h down then in the 20min, obtains multistage hole silicon dioxide granule.
The particle diameter of prepared multistage hole silicon dioxide granule is that 200 ~ 300nm, mesoporous size are about 3nm, porosity is about 80%.
Take by weighing the multistage hole silicon dioxide granule of 0.2g; With ultrasonic cell disruptor it is dispersed in the 40mL toluene solution that contains 0.377mL ten difluoro heptyl propyl trimethoxy siloxanes; Under 80 ℃, back flow reaction 8h, with toluene wash and centrifugal to ten difluoro heptyl propyl trimethoxy siloxanes remove clean till; Temperature is 80 ℃ of dry 24h down, obtains the multistage hole silicon dioxide granule of modification.
Take by weighing the multistage hole silicon dioxide granule of 0.2g modification, be dispersed in 1.8gC
12Alkane and 4.2gC
14In the mixture of alkane, be under the 0.09MPa in vacuum tightness, continuously stirring is adsorbed organic alkane phase change material 4h; Whip attachment 12h under normal pressure then; Stop absorption, centrifugal twice with toluene wash, obtain the organic alkane phase change material of multistage hole silicon dioxide granule load.
Measure charge capacity with anti-STA 449 C that speed of Germany, recording the machine alkane charge capacity that loads in the multistage hole silicon-dioxide is 12.6% of silicon-dioxide quality.
The multistage hole silicon dioxide granule of the organic alkane phase change material of 0.12g load is dispersed in the 2g toluene with ultrasonic cell pulverization machine; The silicone resin uniform mixing that is heating and curing with 2g then; Be coated on 3cm * 3cm aluminium sheet, solidify 30min down at 30 ℃, 75 ℃ solidify 45min down; Solidify 2h down at 150 ℃ again, obtain the anti-icing coating of the multistage hole silicon dioxide granule of the organic alkane phase change material of load.
More than the present invention has been done exemplary description; Should be noted that; Under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (3)
1. a silicon dioxide carried organic alkane phase change material is characterized in that, this phase change material be with particle diameter be 10 ~ 800nm, to have porosity be that 30 ~ 80% hollow silicon dioxide granule mesoporous or multistage hole is a carrier, load C
10~ C
16Organic alkane, organic alkane of its load is 10% ~ 13% of silicon-dioxide quality.
2. preparation method by the described silicon dioxide carried organic alkane phase change material of claim 1 is characterized in that may further comprise the steps:
1) preparation of silicon dioxide granule
Method one: in volumetric concentration was 20 ~ 60% aqueous ethanolic solution, temperature was that 25wt% ammoniacal liquor volume ratio is (0.5 ~ 1.5) by tetraethoxy and concentration: 1 at 10 ~ 30 ℃; Cationic emulsifier hexadecyl trimethoxy brometo de amonio and tetraethoxy mass ratio are 1: (5 ~ 15); At first in aqueous ethanolic solution, add cationic emulsifier hexadecyl trimethoxy brometo de amonio, stirring velocity is under 500 ~ 1000rpm, drips tetraethoxy; Emulsification 5 ~ 15mim; Adding concentration then is 25wt% ammoniacal liquor, and reaction 1 ~ 5h is dried 12 ~ 24h down through the throw out that spinning obtains for 60 ~ 80 ℃ in temperature; Be elevated to 300 ~ 600 ℃ of calcining 3 ~ 6h down then in the 20min, obtain hollow mesoporous silicon oxide particle;
Method two: in the mixing solutions of ether, ethanol, deionized water volume ratio 1:2:7, temperature is that 25wt% ammoniacal liquor volume ratio is (3 ~ 7) by tetraethoxy and concentration: 1 at 10 ~ 30 ℃; Cationic emulsifier hexadecyl trimethoxy brometo de amonio and tetraethoxy mass ratio are 1: (1 ~ 5); At first in mixing solutions, add emulsifying agent hexadecyl trimethoxy brometo de amonio, stirring velocity is under 500 ~ 1000rpm, drips tetraethoxy; Emulsification 5 ~ 15mim; Adding concentration then is 25wt% ammoniacal liquor, and reaction 1 ~ 5h is dried 12 ~ 24h down through the throw out that spinning obtains for 60 ~ 80 ℃ in temperature; Be elevated to 300 ~ 600 ℃ of calcining 3 ~ 6h down then in the 20min, obtain multistage hole silicon dioxide granule;
2) modification of the silicon dioxide granule that makes of step 1)
The mol ratio of pressing the coupling agent of silicon dioxide granule and ten difluoro heptyl propyl trimethoxy siloxanes is (2 ~ 4): 1; Be dispersed in silicon dioxide granule in the toluene solution that contains ten difluoro heptyl propyl trimethoxy siloxanes with the cell pulverization machine; Atmospheric pressure reflux reaction 5 ~ 10h under 50 ~ 100 ℃ of temperature; Collect phegma; Till removing totally with toluene wash is also centrifugal to ten difluoro heptyl propyl trimethoxy siloxanes,, obtain the mesoporous or multistage hole silicon dioxide granule of silane coupler modified hollow at 50 ~ 90 ℃ of down dry 12 ~ 24h of temperature;
3) silicon dioxide carried organic alkane phase change material
Silicon dioxide granule and organic alkane C of the modification that set by step 2) makes
10~ C
16Mass ratio be (0.02 ~ 0.2): 1; The improved silica particle is added in organic alkane, is under 0.01MPa ~ 0.1MPa in vacuum tightness, and continuously stirring is adsorbed organic alkane phase change material 1 ~ 10h; Whip attachment 10 ~ 20h under normal pressure then; Use toluene wash, spinning again, remove the organic alkane that is adsorbed on silica particle surface, obtain silicon dioxide carried organic alkane phase change material.
3. described by claim 1 or press the prepared silicon dioxide carried organic alkane phase change material of claim 2 application: this silicon dioxide carried organic alkane phase change material and silicone resin are compound, are applied to anti-icing coated material.
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