CN101480596A - Method for preparing phase-change energy-storage nano capsule powder and use thereof - Google Patents
Method for preparing phase-change energy-storage nano capsule powder and use thereof Download PDFInfo
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- CN101480596A CN101480596A CNA2008102024043A CN200810202404A CN101480596A CN 101480596 A CN101480596 A CN 101480596A CN A2008102024043 A CNA2008102024043 A CN A2008102024043A CN 200810202404 A CN200810202404 A CN 200810202404A CN 101480596 A CN101480596 A CN 101480596A
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Abstract
The invention relates to a method for preparing phase change nanometer capsule powder. The method comprises the following steps: firstly, phase change materials are fused with monomers subjected to polymerization, and the mixture is mixed with aqueous solution of an emulsion agent by mechanical stirring; secondly, the mixture is subjection to fine emulsification to break up an oil phase into small oil drops which are dispersed into water to form fine miniemulsion; thirdly, an initiating agent initiates monomers in the miniemulsion to polymerize, and the generated polymer is incompatible with the phase materials and is gradually separated to form the capsule emulsion of encapsulation phase change materials; according to the emulsion breaking principle, nanometer capsules made of the phase change materials are separated out, the impurities of the nanometer capsules are removed, and the nanometer capsules are naturally dried or baked at low temperature to obtain nanometer capsule powder materials made of the phase change materials. The phase change nanometer capsule powder prepared by the method has the following steps: (1) the latent heat is large and the heat conduction coefficient is high; (2) the particle diameter is small, so the phase change nanometer capsule powder is irreplaceable in the field of electronic heat dissipation micro-channels; and (3) encapsulation phase change materials cannot flow out when undergoing the phase change and can be applied in the fields of dope, textile, and the like.
Description
Technical field
The invention belongs to the material field, relate to energy-storage composite material, especially phase-change energy-storage nano capsule powder and preparation method thereof.
Background technology
Particularly microelectron-mechanical (MEMS) technical development was very swift and violent in recent years, and expanded gradually in a plurality of application scenarios, and microminaturization has become one of important directions of contemporary science and technology development.Miniature refrigerating technology had both depended on the development of MEMS technology, also was the needs of MEMS technical development simultaneously.As everyone knows, the fast development of integrated circuit technique causes the volume of various electronic devices and product more and more littler, and the heat flow density around the integrated device is increasing, with the computer CPU is example, and the heat flow density that produces in its running has reached 60-100W/cm
2, in the semiconductor laser even reach 103W/cm
2The order of magnitude.On the other hand, the reliability of electronic device work is but very responsive to temperature, device temperature 1 ℃ of every increase on 70-80 ℃ of level, and reliability will descend 5%; If increase by 10～20 ℃, then fault rate improves 100%.Higher temperature levels becomes restriction electronic device bottleneck of performance day by day, and the control of the temperature of efficent electronic device has become a research focus at present gradually.
In the electronic element radiating technical field, generally adopt organic matter at present, and, stable performance big with storage density and lower-cost paraffin are used at most as phase-change material.But the thermal conductivity factor that paraffin is low has seriously restricted the heat transfer property of heat-storing device, has new departure to rely on the raising of thermal conductivity factor to improve rate of heat transfer.But because powder body material density is usually greater than paraffin, so compound tense is difficult to form the phase-change material of homogeneous; On the other hand, do not have direct active force between powder (comprising foam metal) and paraffin, in its melt temperature zone, paraffin can be separated between its hole or powder particle.Some scholar proposes microencapsulated phase change material, but its thermal conductivity factor is very low, has reduced the heat transfer property between heating electronic device and cooling system, and size ratio is bigger, thereby easy blocking pipe.New departure remains to be proposed to address this problem better.
Summary of the invention
The object of the present invention is to provide a kind of phase-change energy-storage nano capsule powder and preparation method thereof, this Nano capsule material not only can improve the heat conductivility of material greatly, and because its particle diameter is enough little, can be applied to field widely.
At the requirement of fields such as electronic radiation to phase-changing energy storage material, the present invention adopts fine emulsion polymerization to prepare a kind of phase-change energy-storage nano capsule powder material,
The principle of the invention: phase-change material at first merges with the monomer that polymerization takes place, and mixes with emulsifier aqueous solution liquid then, mixes through mechanical agitation.Through thin emulsification, oil phase is dispersed as tiny oil droplet is scattered in the aqueous solution then, form miniemulsion.At a certain temperature, initator causes the monomer polymerization in the miniemulsion, and the polymer and the phase-change material of generation are incompatible, separates gradually, forms the capsule emulsion of coating phase-change materials.According to emulsion breaking principle, the phase-change material Nano capsule is separated, remove impurity, oven dry can obtain phase-change material nano capsule powder material under the low temperature.
Concrete preparation method is as follows.
(1) material selecting for use and handling.
The selection of material:
Alkanes (as octadecane Oct, specification is fertile triumphant, and traditional Chinese medicines group in Shanghai produces) is as phase-change material;
Styrene St (chemical pure CP, traditional Chinese medicines group in Shanghai produces) is as the filmogen monomer.
Initator adopts azodiisobutyronitrile AIBN (chemical pure CP, traditional Chinese medicines group in Shanghai produces), perhaps potassium peroxydisulfate KPS (chemical pure CP, traditional Chinese medicines group in Shanghai produces);
Co-stabilizer adopts hexadecanol CA (chemical pure CP, traditional Chinese medicines group in Shanghai produces);
Emulsifying agent adopts lauryl sodium sulfate SDS (electronics is pure, and traditional Chinese medicines group in Shanghai produces), perhaps the compound surfactant that combines of SDS and non-ionic surface active agent APES OP-10 (chemical pure CP, the production of Shanghai traditional Chinese medicines group);
Deionized water is between scope 25～40g.
(2) preparation of miniemulsion
Pre-emulsification: according to the experiment proportioning, in a beaker, emulsifying agent (as lauryl sodium sulfate SDS) and assistant for emulsifying agent (as hexadecane HD or hexadecanol CA) are dissolved in the deionized water, and mechanical agitation, it is more even that medicine is mixed.In another beaker, with the monomer of certain proportioning, alkane perhaps also have initator (if oiliness initiator A IBN), and machinery mixes.Proportioning between each composition of miniemulsion is probably as follows: SDS:HD:St:Oct:Water=0.01～0.4g:0.01～2.0:1.0g～5.0g:1.0g～5.0g:25～40g.
Emulsification: emulsifier aqueous solution is poured in the monomer oil phase, further carries out high-speed stirred by magnetic stirrer and mixes, and rotating speed is adjustable.
Thin emulsification: said mixture is passed through the further homogenizing of sonic oscillation, ultrasonic time, and ultrasonic power output how much changing according to the mixture amount.In the operating process of this experiment, limiting ultrasonic time is 1min～15min, and ultrasonic power output is 40%～90% (instrument can be given birth to the KS-600 that produces with Ningbo section) of rated power.
(3) polymerization process
Polyplant is by magnetic stirrer, tank, and there-necked flask, condenser pipe, nitrogen cylinder, constant pressure funnel, wherein magnetic stirrer has the effect of heating temperature control, and magnetic stir bar is all arranged in tank and the flask.Miniemulsion is moved in the there-necked flask, and start the agitating function of magnetic stirrer, feed the nitrogen deoxygenation simultaneously, because oxygen has the side effect of having an effect with free radical and stopping polymerization.After 20～40 minutes, there-necked flask is moved in the tank.Bath temperature is risen to 60～75 degrees centigrade, initiated polymerization (, then needing to splash into initator with constant pressure funnel, initiated polymerization) if that use is water soluble starter KPS.In the course of reaction, nitrogen can not interrupt.React after 4～6 hours, cool off phase transformation capsule emulsion.
(4) capsule powder preparation
The capsule emulsion is if make powder, two steps of needs experience.At first want breakdown of emulsion, the capsule top layer is enclosed with one deck emulsifying agent, capsule need be separated.Then, get rid of the alkane phase-change material that is not wrapped again.At first allocate 5%～15% NaCl solution, and then add 1%～5% ethanol, as the breakdown of emulsion solution of capsule emulsion.Then, the capsule emulsion is splashed in the breakdown of emulsion solution, filter paper filters.At last, splash into petroleum ether solution again, filter once more.Naturally dry under normal temperature, perhaps low temperature drying can make the nano capsule powder material.
Advantage of the present invention: (1) latent heat is big, the thermal conductivity factor height; (2) particle diameter is very little, has the status of not replacing in field, electronic radiation microchannel; (3) coating phase-change materials undergoes phase transition the Shi Buhui outflow, can be applied to coating, fields such as weaving.
Description of drawings
Fig. 1 is the reaction generating means figure of the embodiment of the invention.(wherein: " 1 " is constant pressure funnel, and " 2 " are the constant temperature magnetic stirrer.)
The phase-change material Nano capsule AFM height map that Fig. 2 prepares for the embodiment of the invention.
The phase-change material Nano capsule AFM phase diagram that Fig. 3 prepares for the embodiment of the invention.
The phase-change material Nano capsule AFM graphics that Fig. 4 prepares for the embodiment of the invention.
The phase-change material Nano capsule DSC curve map that Fig. 5 prepares for the embodiment of the invention.
The differential volume distributed median figure of the phase-change material Nano capsule particle diameter that Fig. 6 prepares for the embodiment of the invention.
The specific embodiment
With 2.0g styrene, the 4.0g octadecane, the 0.03g azodiisobutyronitrile is made into oil-phase solution, is added to the 30g deionized water, in the aqueous solution that 0.03g lauryl sodium sulfate and 0.06g hexadecanol are formed.Adopt mechanical agitation 7 minutes earlier, obtain emulsion, adopt ultrasonic cell pulverization then 10 minutes (70% power-handling capability), obtain miniemulsion.Miniemulsion transferred to be equipped with return duct, nitrogen inlet, charge door, volume are in the there-necked flask of 1L, stir earlier, logical nitrogen deoxygenation is after 40 minutes, under the return duct condensation, nitrogen continues uninterrupted, and bath temperature reaches 68 degrees centigrade, reacted five hours, cooling obtains phase transformation Nano capsule emulsion naturally.Phase transformation capsule emulsion is transferred in the solution of being made up of 10%NaCl concentration and 2% ethanol, and breakdown of emulsion filters to isolate the phase transformation Nano capsule.Drip petroleum ether solution and soak the filtration of phase transformation Nano capsule, dry naturally or low temperature (below 24 degrees centigrade) oven dry, promptly make phase transformation nano capsule powder material.
With 2.4g styrene, the 3.6g octadecane, the 0.03g azodiisobutyronitrile is made into oil-phase solution, is added to the 30g deionized water, in the aqueous solution that 0.25g lauryl sodium sulfate and 0.06g hexadecanol are formed.Adopt mechanical agitation 7 minutes earlier, obtain emulsion, adopt ultrasonic cell pulverization then 12 minutes (68% power-handling capability), obtain miniemulsion.Miniemulsion transferred to be equipped with return duct, nitrogen inlet, charge door, volume are in the there-necked flask of 1L, stir earlier, logical nitrogen deoxygenation is after 30 minutes, under the return duct condensation, nitrogen continues uninterrupted, and bath temperature reaches 68 degrees centigrade, reacted five hours, cooling obtains phase transformation Nano capsule emulsion naturally.Phase transformation capsule emulsion is transferred in the solution of being made up of 10%NaCl concentration and 3% ethanol, and breakdown of emulsion filters to isolate the phase transformation Nano capsule.Drip petroleum ether solution and soak the filtration of phase transformation Nano capsule, dry naturally or low temperature (below 24 degrees centigrade) oven dry, promptly make phase transformation nano capsule powder material.
Embodiment 3
With 3.0g styrene, the 3.0g octadecane, the 0.03g azodiisobutyronitrile is made into oil-phase solution, is added to the 30g deionized water, and the 0.13g lauryl sodium sulfate is in the aqueous solution that 0.12g APES and 0.06g hexadecanol are formed.Adopt mechanical agitation 7 minutes earlier, obtain emulsion, adopt ultrasonic cell pulverization then 15 minutes (40% power-handling capability), obtain miniemulsion.Miniemulsion transferred to be equipped with return duct, nitrogen inlet, charge door, volume are in the there-necked flask of 1L, stir earlier, logical nitrogen deoxygenation is after 35 minutes, under the return duct condensation, nitrogen continues uninterrupted, and bath temperature reaches 68 degrees centigrade, reacted five hours, cooling obtains phase transformation Nano capsule emulsion naturally.Phase transformation capsule emulsion is transferred in the solution of being made up of 10%NaCl concentration and 5% ethanol, and breakdown of emulsion filters to isolate the phase transformation Nano capsule.Drip petroleum ether solution and soak the filtration of phase transformation Nano capsule, dry naturally or low temperature (below 24 degrees centigrade) oven dry, promptly make phase transformation nano capsule powder material.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (5)
1, a kind of preparation method of phase-change energy-storage nano capsule powder, it is characterized in that: the method that is adopted is a fine emulsion polymerization.
2, the preparation method of phase-change energy-storage nano capsule powder according to claim 1 is characterized in that: at first the monomer with phase-change material and generation polymerization merges, and mixes with emulsifier aqueous solution liquid then, mixes through mechanical agitation; Through thin emulsification, oil phase is dispersed as tiny oil droplet is scattered in the aqueous solution then, form miniemulsion; Initator causes the monomer polymerization in the miniemulsion, and the polymer and the phase-change material of generation are incompatible, separates gradually, forms the capsule emulsion of coating phase-change materials; According to emulsion breaking principle, the phase-change material Nano capsule is separated, remove impurity, in dry naturally under the normal temperature or low temperature under oven dry can obtain phase-change material nano capsule powder material.
3, the preparation method of phase-change energy-storage nano capsule powder according to claim 1 is characterized in that: comprising:
(1) material selecting for use and handling
The selection of material:
With alkanes as phase-change material;
With styrene St as the filmogen monomer; Initator adopts azodiisobutyronitrile AIBN or potassium peroxydisulfate KPS;
Co-stabilizer adopts hexadecanol CA;
The compound surfactant that emulsifying agent adopts lauryl sodium sulfate SDS or SDS to combine with non-ionic surface active agent APES OP-10;
Deionized water is between scope 25～40g;
(2) preparation of miniemulsion
Pre-emulsification: according to the experiment proportioning, in a beaker, emulsifying agent and assistant for emulsifying agent are dissolved in the deionized water, and mechanical agitation, it is more even that medicine is mixed; In another beaker, with the monomer of certain proportioning, alkane, perhaps if oiliness initiator A IBN then also has initator, and machinery mixes;
Emulsification: emulsifier aqueous solution is poured in the monomer oil phase, further carries out high-speed stirred by magnetic stirrer and mixes, and rotating speed is adjustable;
Thin emulsification: said mixture is passed through the further homogenizing of sonic oscillation, ultrasonic time, and ultrasonic power output how much changing according to the mixture amount;
(3) polymerization process
Miniemulsion is moved in the there-necked flask, and start the agitating function of magnetic stirrer, feed the nitrogen deoxygenation simultaneously, initiated polymerization after 20～40 minutes; In the course of reaction, nitrogen does not interrupt; After the reaction, cool off phase transformation capsule emulsion;
(4) capsule powder preparation
The capsule emulsion is made powder, and the experience following steps: at first want breakdown of emulsion, the capsule top layer is enclosed with one deck emulsifying agent, capsule need be separated; Then, get rid of the alkane phase-change material that is not wrapped again, last, under normal temperature, dry naturally or low temperature drying, can make the nano capsule powder material.
4, the preparation method of phase-change energy-storage nano capsule powder according to claim 3 is characterized in that:
In the selecting for use and handle of material, with octadecane Oct as phase-change material;
In the preparation of miniemulsion, emulsifying agent adopts lauryl sodium sulfate SDS, and assistant for emulsifying agent adopts hexadecane HD or hexadecanol CA; Proportioning between each composition of miniemulsion is as follows: SDS:HD:St:Oct:Water=0.01～0.4g:0.01～2.0:1.0g～5.0g:1.0g～5.0g:25～40g;
In the thin emulsion process, limiting ultrasonic time is 1min～15min, and ultrasonic power output is 40%～90% of a rated power;
In the polymerization process,
Described magnetic stirrer has the effect of heating temperature control, and magnetic stir bar is all arranged in tank and the flask; Miniemulsion is moved in the there-necked flask, and start the agitating function of magnetic stirrer, feed the nitrogen deoxygenation simultaneously, after 20～40 minutes, there-necked flask is moved in the tank; Bath temperature is risen to 60～75 degrees centigrade, and initiated polymerization if that perhaps use is water soluble starter KPS, then needs to splash into initator with constant pressure funnel, initiated polymerization; React after 4～6 hours, cool off phase transformation capsule emulsion;
In the capsule powder preparation process,
At first allocate 5%～15% NaCl solution, and then add 1%～5% ethanol, as the breakdown of emulsion solution of capsule emulsion; Then, the capsule emulsion is splashed in the breakdown of emulsion solution, filter paper filters; At last, splash into petroleum ether solution again, filter once more; Under normal temperature, dry naturally or low temperature drying, can make the nano capsule powder material.
5, according to the application of the phase-change energy-storage nano capsule powder of the described method of claim 1-4 preparation at microelectron-mechanical, coating and field of textiles.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103801240A (en) * | 2014-02-27 | 2014-05-21 | 盐城工学院 | Method for preparing phase-change nano capsule at room temperature |
| CN105969316A (en) * | 2016-06-03 | 2016-09-28 | 宁海德宝立新材料有限公司 | Phase-change heat-storage composite material for hot compress |
| CN106629590A (en) * | 2017-01-13 | 2017-05-10 | 北京林业大学 | Preparation method of novel ZIF-8 (Zeolitic Imidazolate Framework-8) clad n-octadecane phase-change gas-storage material |
| CN107903876A (en) * | 2017-11-09 | 2018-04-13 | 中国皮革和制鞋工业研究院 | A kind of phase-change microcapsule and its preparation method and application |
| CN108053962A (en) * | 2017-11-15 | 2018-05-18 | 宁波大学科学技术学院 | A kind of heat accumulation magnetic material of shell-like structure and preparation method thereof |
| CN109913177A (en) * | 2019-03-04 | 2019-06-21 | 河北工业大学 | Double phase-change accumulation energy automatically cleaning materials for walls and its application |
| CN112961600A (en) * | 2021-03-22 | 2021-06-15 | 广东希贵光固化材料有限公司 | EB (Electron Beam) -cured copper-clad aluminum substrate heat-dissipating coating |
| CN113072871A (en) * | 2021-03-22 | 2021-07-06 | 广东希贵光固化材料有限公司 | EB (Electron Beam) curing cigarette end burning resistant coating |
| CN113321989A (en) * | 2021-06-02 | 2021-08-31 | 广东希贵光固化材料有限公司 | Insulation heat dissipation coating for EB (Electron Beam) cured aluminum-based copper-clad plate |
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- 2008-11-07 CN CNA2008102024043A patent/CN101480596A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103801240A (en) * | 2014-02-27 | 2014-05-21 | 盐城工学院 | Method for preparing phase-change nano capsule at room temperature |
| CN103801240B (en) * | 2014-02-27 | 2016-02-17 | 盐城工学院 | Normal temperature prepares the method for phase transformation Nano capsule |
| CN105969316A (en) * | 2016-06-03 | 2016-09-28 | 宁海德宝立新材料有限公司 | Phase-change heat-storage composite material for hot compress |
| CN106629590A (en) * | 2017-01-13 | 2017-05-10 | 北京林业大学 | Preparation method of novel ZIF-8 (Zeolitic Imidazolate Framework-8) clad n-octadecane phase-change gas-storage material |
| CN107903876A (en) * | 2017-11-09 | 2018-04-13 | 中国皮革和制鞋工业研究院 | A kind of phase-change microcapsule and its preparation method and application |
| CN108053962A (en) * | 2017-11-15 | 2018-05-18 | 宁波大学科学技术学院 | A kind of heat accumulation magnetic material of shell-like structure and preparation method thereof |
| CN109913177A (en) * | 2019-03-04 | 2019-06-21 | 河北工业大学 | Double phase-change accumulation energy automatically cleaning materials for walls and its application |
| CN112961600A (en) * | 2021-03-22 | 2021-06-15 | 广东希贵光固化材料有限公司 | EB (Electron Beam) -cured copper-clad aluminum substrate heat-dissipating coating |
| CN113072871A (en) * | 2021-03-22 | 2021-07-06 | 广东希贵光固化材料有限公司 | EB (Electron Beam) curing cigarette end burning resistant coating |
| CN113072871B (en) * | 2021-03-22 | 2022-05-06 | 广东希贵光固化材料有限公司 | EB (Electron Beam) curing cigarette end burning resistant coating |
| CN113321989A (en) * | 2021-06-02 | 2021-08-31 | 广东希贵光固化材料有限公司 | Insulation heat dissipation coating for EB (Electron Beam) cured aluminum-based copper-clad plate |
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