CN1900209A - Process for preparing nano capsule phase change material emulsion - Google Patents
Process for preparing nano capsule phase change material emulsion Download PDFInfo
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- CN1900209A CN1900209A CN 200610036494 CN200610036494A CN1900209A CN 1900209 A CN1900209 A CN 1900209A CN 200610036494 CN200610036494 CN 200610036494 CN 200610036494 A CN200610036494 A CN 200610036494A CN 1900209 A CN1900209 A CN 1900209A
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Abstract
The process of preparing nanometer capsule phase change material emulsion includes adding the oil phase liquid compounded with olefin monomer, hydrophilic monomer, alkane, initiator and n-lauryl mercaptan into the mixed liquid of emulsifier and deionized water via stirring and ultrasonic dispersing to obtain micro emulsion, introducing nitrogen to the micro emulsion system to eliminate oxygen via stirring, reflux condensing, heating to 65 deg.c and constant temperature polymerization reaction for 5 hr, and cooling naturally to room temperature to obtain the nanometer capsule phase change material emulsion. Thus prepared nanometer capsule phase change material emulsion has nanometer size, stable performance, great phase change enthalpy and wide application in latent heat functional hot fluid, heat accumulating and temperature regulating fabric, energy saving building wall and other fields.
Description
Technical field
The present invention relates to a kind of preparation method of phase change material, particularly a kind of preparation method of nano capsule phase change material emulsion.
Background technology
Potential heat functional thermal fluid (Latent functionally thermal fluid, LFTF) heat-transfer fluid for having specific function.It is to utilize phase change material particulate (being generally capsule) to absorb or discharge the reinforcement that latent heat is realized heat transfer process in phase transition process.Compare with common single-phase heat transfer fluid, LFTF has very big apparent specific heat, can obviously increase the heat-transfer capability between heat-transfer fluid and runner wall, is a kind of novel materials that integrates heat accumulation and enhancement of heat transfer function.It not only can be used as the efficient heat transfer medium, big spoke degree improves effective specific heat of fluidic and heat transfer property, significantly reduce the size of interchanger and cold fluid and hot fluid transport pipe, reduce it and carry power consumption, and can be used as the accumulation of energy medium, be used for various heat storage and cold accumulation system, realize energy storage and transport medium integrated, alleviate energy supply and demand both sides unmatched contradiction on time and intensity, in heating, air-conditioning and field of heat exchangers, application prospect is boundless.
Among the LFTF commonly used, the capsular particle diameter of phase change material is in μ m magnitude, but in the actual use, there is the deficiency of following aspect in discovery: because particle diameter is bigger, fluidic viscosity height causes the pump consumption to increase (1); (2) capsule grain diameter is bigger, increases because of the collision of particle and pump wall makes capsule conquassation, damaged probability in the pumping process, makes fluidic stability reduce; (3) capsule grain diameter is bigger, and specific surface area is low, and the thermal conduction probability reduces between particle.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the emulsion preparation method of the nano capsule phase change material that a kind of particle size is nano level, stable performance, enthalpy of phase change is bigger is provided.
The emulsion preparation method of nano capsule phase change material of the present invention, may further comprise the steps: vinyl monomer, the common monomer of wetting ability, alkane, initiator and positive Dodecyl Mercaptan are made into oil phase liquid join in the mixed solution of emulsifying agent and deionized water, mechanical stirring 10min, ultra-sonic dispersion 15min obtains microemulsion again, microemulsion is stirred, leads to nitrogen 30min remove system oxygen, then under reflux condensation mode, heat temperature raising to 65 ℃, polyreaction 5h under 65 ℃ of constant temperature, reaction finishes and naturally cools to room temperature and can obtain nano capsule phase change material emulsion of the present invention; Described vinyl monomer, the wetting ability mass fraction of monomer, alkane, initiator and positive Dodecyl Mercaptan consumption altogether are:
Vinyl monomer 100,
Alkane 66～150,
Wetting ability is monomer 3～6 altogether,
Initiator 0.6～2,
Positive Dodecyl Mercaptan 1～3,
Emulsifying agent 1.5～4.5.
Preferred version is as follows:
Selected vinyl monomer is vinylbenzene or alpha-methyl styrene or methyl methacrylate;
Selected alkane is that carbonatoms is 16～27 normal paraffin or paraffin, and vinyl monomer can be compatible with alkane;
Described wetting ability monomer altogether is methacrylic acid (MAA) or butyl acrylate (BA);
Described initiator is water-soluble or oil-soluble initiator, is azo-bis-isobutyl cyanide preferably;
Described emulsifying agent is that anionic emulsifier sodium lauryl sulphate (SDS) and/or nonionic emulsifying agent are appointed basic phenol polyoxyethylene ether (OP-10), and its consumption is 0～2: 0～1 weight, and both are not 0 simultaneously.
Principle of work of the present invention is as follows: vinyl monomer had both been made reaction monomers, make the alkane good solvent again, the normal paraffin phase change material is dissolved in and wherein forms oil phase liquid, because cavitation effect of ultrasonic waves, oil phase liquid is dispersed as nano-liquid droplet, then under the emulsifying agent effect, formation is the microemulsion of external phase with water, behind the initiated polymerization, oil phase monomer droplet " on the spot " granulating, because the polymkeric substance and the alkane that generate are incompatible, be separated in the micelle, the formation polymkeric substance is shell, the capsule structure of alkane for examining.By the ultrasonic emulsifying process that involves, can control capsular size in nanometer range, thereby obtain nano capsule phase change material emulsion.
Employed alkane is because the carbonatoms difference among the present invention, and if the fusing point difference when selecting higher alkane of carbonatoms such as paraffin for use, needs the vinyl monomer water bath with thermostatic control is heated to 40 ℃, adds melt paraffin then and is dissolved in vinyl monomer; The wetting ability that is adopted altogether monomer is used to improve the fragility of alkene monomer polymer, reduces the surface tension of monomer and water termination, helps forming the packing structure, the stability of increase Nano capsule in water miscible liquid; The positive Dodecyl Mercaptan that is adopted is used to make polymeric chain to shorten as chain-transfer agent, and the chain movability increases, and the degree that is separated increases, thus control capsule grain diameter size and form; The initiator that is adopted is used for forming smoothly ball-type capsule.The present invention fed high pure nitrogen 30min earlier before polyreaction, prevent that the oxygen in the system from catching the radical in the initiator and making its reaction inactivation.
The present invention has following advantage and effect with respect to prior art: (1) latent heat amount is big, accumulation of energy and good heat-transfer; (2) capsule grain diameter is little, and fluid viscosity is low, can significantly reduce the fluid pumping resistance, and the pump consumption is low.(3) capsule grain diameter is little, and is evenly dispersed, and stability is high.(4) material of the present invention's preparation can be applicable in fields such as potential heat functional thermal fluid, heat-accumulation temperature-adjustment textiles and building energy conservation bodies of wall.
Description of drawings
Fig. 1 is nano capsule phase change material transmission electron microscope (TEM) figure,
Fig. 2 is nano capsule phase change material differential scanning calorimetric (DSC) figure,
Fig. 3 is nano capsule phase change material size distribution figure.
Embodiment
Below in conjunction with body embodiment and accompanying drawing the present invention is further described, but of the present inventionly is not limited to this.
Embodiment 1
The oil phase liquid that 30g vinylbenzene, 30g fusion Octadecane, 0.9g butyl acrylate, 0.3g Diisopropyl azodicarboxylate and the positive Dodecyl Mercaptan of 0.4g are made into, join 1.2g compound emulsifying agent (SDS: OP-10=1: 1) in the solution of forming with the 240g deionized water, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir, lead to nitrogen 30min earlier to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature and make nano capsule phase change material.
30g vinylbenzene, 45g fusion Octadecane, 1.2g vinylformic acid, 0.4g Diisopropyl azodicarboxylate and the positive Dodecyl Mercaptan of 0.6g are made into oil phase liquid, join in the solution of 1.2gSDS and 240g deionized water composition, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 3
30g methyl methacrylate, 40g fusion NSC 62789,0.9g butyl acrylate and the positive Dodecyl Mercaptan of 0.9g are made into oil phase liquid, join in the solution of 0.6g Potassium Persulphate, 1.2gSDS and 240g deionized water composition, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 4
The oil phase liquid that 30g alpha-methyl styrene, 30g fusion NSC 62789,1.5g vinylformic acid and the positive Dodecyl Mercaptan of 0.45g are made into, join 0.4g ammonium persulphate, 1.35g compound emulsifying agent (SDS: OP-10=2: 1) in the solution of forming with the 240g deionized water, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 5
Under 40 ℃ of water-baths, with 30g vinylbenzene, 30g melt paraffin (45 ℃ of fusing points), 0.6g Diisopropyl azodicarboxylate, 1.2g the oil phase liquid that the positive Dodecyl Mercaptan of vinylformic acid and 0.8g is made into, join 1.2g compound emulsifying agent (SDS: OP-10=1: 1) in the solution of forming with the 240g deionized water, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 6
30g vinylbenzene, 20g fusion Octadecane, 1.2g butyl acrylate, 0.5g Diisopropyl azodicarboxylate and the positive Dodecyl Mercaptan of 0.6g are made into oil phase liquid, join in the solution of 1.2g OP-10 and 240g deionized water composition, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 7
30g vinylbenzene, 45g fusion n-hexadecane, 1.8g vinylformic acid, 0.6g Diisopropyl azodicarboxylate and the positive Dodecyl Mercaptan of 0.9g are made into oil phase liquid, join 1.35g (SDS: OP-10=1: 1) in the solution of forming with the 240g deionized water, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
Embodiment 8
Under 40 ℃ of water-baths, 30g methyl methacrylate, 20g melt paraffin (45 ℃ of fusing points), 1.2g butyl acrylate, 0.6g Diisopropyl azodicarboxylate and the positive Dodecyl Mercaptan of 0.3g are made into oil phase liquid, join 0.6g (SDS: OP-10=1: 1) in the solution of forming with the 240g deionized water, adopt mechanical stirring 10min to obtain emulsion earlier, obtain microemulsion with the ultrasonic 15min of ultrasonic cell disruptor then.Microemulsion changed over to be equipped with return line, nitrogen inlet, in the 500ml four-hole boiling flask of mechanical stirring and charging opening, stir earlier, lead to nitrogen 30min to remove system oxygen, then under the return line condensation, heat temperature raising to 65 ℃ water bath with thermostatic control polyreaction 5h, reaction finishes and naturally cools to room temperature.
The performance introduction of the nano capsule phase change material of the present invention's preparation is as follows:
Nano capsule phase change material to embodiment 1,2 preparations carries out performance analysis, and its TEM figure (amplifies 70,000 times) as described in Figure 1, and its DSC schemes as shown in Figure 2, and its size distribution figure as shown in Figure 3.
Fig. 1 shows that the synthetic material is tangible capsule structure, and the aggregation features according to reaction can draw, and external bladder wall part (dark color) is an olefin polymer, and capsule-core part (light color) is the alkane phase change material.Its size-grade distribution is comparatively regular, and shape is spherical in shape, and grain size shows that prepared capsule is comparatively uniform nanometer spherical particle about 100nm.
Fig. 2 shows, adopts alkane to make phase change material (octadecane), has sizable latent heat enthalpy (231.7kJ/kg), and behind micro encapsulation, its enthalpy of phase change reduces, but still has higher enthalpy of phase change.As embodiment 1 (alkane/vinyl monomer ratio is 1/1), its enthalpy of phase change is 125.7kJ/kg, and along with alkane content in the capsule increases (embodiment 2, and alkane/vinyl monomer ratio is 3/2), its phase transformation enthalpy (134.4kJ/kg) increases.With pure octadecane relatively, that their transformation temperature changes is very little (corresponding to about 28 ℃ of the fusing points of alkane); And capsule and pure octadecane phase transformation enthalpy ratio, corresponding to alkane content in capsule.This shows, just capsule-core alkane phase change material is shielded, prevent the leakage of phase change material in phase transition process, and cyst wall is to the not influence of hot rerum natura of capsule-core as the alkene monomer polymer of cyst wall.
Fig. 3 shows, the capsular size of phase change material (peak value) about 100nm of embodiment 1 preparation, and its narrower particle size distribution shows that capsule grain diameter is comparatively even, its test result is consistent with the result of transmission electron microscope (Fig. 1).The capsule phase change material of different alkane/vinyl monomer proportioning, along with the increase of ratio, its particle size slightly increases.As embodiment 1 (proportioning 1/1), its median size is at 137.2nm, and peak value is 91.58nm, and after proportioning increases (embodiment 2), its median size is at 161.3nm, and peak value is 107.2nm.
Claims (6)
1. the preparation method of a nano capsule phase change material emulsion, it is characterized in that comprising: vinyl monomer, the common monomer of wetting ability, alkane, initiator and positive Dodecyl Mercaptan are made into oil phase liquid join in the mixed solution of emulsifying agent and deionized water, stir, ultra-sonic dispersion obtains microemulsion, microemulsion is stirred, leads to nitrogen remove system oxygen, then under reflux condensation mode, heat temperature raising to 65 ℃, polyreaction is 5 hours under 65 ℃ of constant temperature, and reaction finishes and naturally cools to room temperature and can obtain nano capsule phase change material emulsion of the present invention; Described vinyl monomer, the wetting ability mass fraction of monomer, alkane, initiator and positive Dodecyl Mercaptan consumption altogether are:
Vinyl monomer 100,
Alkane 66～150,
Wetting ability is monomer 3～6 altogether,
Initiator 0.6～2,
Positive Dodecyl Mercaptan 1～3,
Emulsifying agent 1.5～4.5.
2. method according to claim 1 is characterized in that selected vinyl monomer is vinylbenzene, alpha-methyl styrene or methyl methacrylate.
3. method according to claim 1 is characterized in that selected employed alkane comprises that carbonatoms is 16～27 the normal paraffin or the mixture of different carbon atom normal paraffins.
4. method according to claim 1 is characterized in that it is methacrylic acid or butyl acrylate that described wetting ability is total to monomer.
5. method according to claim 1 is characterized in that described initiator is water-soluble for ammonium persulphate, Potassium Persulphate or oil-soluble initiator azo-bis-isobutyl cyanide.
6. method according to claim 1, it is characterized in that described emulsifying agent is that anionic emulsifier sodium lauryl sulphate (SDS) and/or nonionic emulsifying agent are appointed basic phenol polyoxyethylene ether (OP-10), its consumption is 0～2: 0～1 weight, and both are not 0 simultaneously.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101838520A (en) * | 2010-04-28 | 2010-09-22 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| CN103801240A (en) * | 2014-02-27 | 2014-05-21 | 盐城工学院 | Method for preparing phase-change nano capsule at room temperature |
| CN108530768A (en) * | 2018-04-27 | 2018-09-14 | 西南科技大学 | Phase transformation latex 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 |
| CN114438614A (en) * | 2021-12-25 | 2022-05-06 | 江苏集萃先进纤维材料研究所有限公司 | Preparation method and product of warm-keeping regenerated cellulose fiber |
| CN115287044A (en) * | 2021-05-04 | 2022-11-04 | 纳米及先进材料研发院有限公司 | Rupture-resistant and easy-to-disperse nano-capsule phase change material and synthesis method thereof |
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| CN1200028C (en) * | 2002-04-22 | 2005-05-04 | 复旦大学 | Polyasparamide derivative and process for preparing its nano capsules |
| CN1491551A (en) * | 2003-09-24 | 2004-04-28 | 河北科技大学 | Ivermectin water suspension nano capsule prepn and its preparing method |
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- 2006-07-14 CN CN2006100364944A patent/CN1900209B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838520A (en) * | 2010-04-28 | 2010-09-22 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| CN101838520B (en) * | 2010-04-28 | 2012-10-17 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| 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 |
| CN108530768A (en) * | 2018-04-27 | 2018-09-14 | 西南科技大学 | Phase transformation latex and preparation method thereof |
| CN108530768B (en) * | 2018-04-27 | 2021-05-07 | 西南科技大学 | Phase-change latex 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 |
| CN115287044A (en) * | 2021-05-04 | 2022-11-04 | 纳米及先进材料研发院有限公司 | Rupture-resistant and easy-to-disperse nano-capsule phase change material and synthesis method thereof |
| CN114438614A (en) * | 2021-12-25 | 2022-05-06 | 江苏集萃先进纤维材料研究所有限公司 | Preparation method and product of warm-keeping regenerated cellulose fiber |
| CN114438614B (en) * | 2021-12-25 | 2023-12-22 | 江苏集萃先进纤维材料研究所有限公司 | Preparation method and product of warm regenerated cellulose fiber |
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