CN102492397B - Preparation method of microencapsulated phase change material with high phase change latent heat value - Google Patents
Preparation method of microencapsulated phase change material with high phase change latent heat value Download PDFInfo
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- CN102492397B CN102492397B CN201110380869.XA CN201110380869A CN102492397B CN 102492397 B CN102492397 B CN 102492397B CN 201110380869 A CN201110380869 A CN 201110380869A CN 102492397 B CN102492397 B CN 102492397B
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Abstract
The invention relates to a preparation method of a microencapsulated phase change material with a high phase change latent heat value. The method comprises: preparing an erythritol solution with erythritol, deionized water, diethylenetriamine, polysorbate-80 and span-80, dissolving isocyanate in liquid paraffin oil so as to obtain an isocyanate solution, adding the erythritol solution into liquid paraffin oil dropwisely so as to obtain a water-in-oil emulsion, and adding the isocyanate solution into the water-in-oil emulsion in a dropwise manner for reaction, then conducting filtration, and drying a solid, thus obtaining a product. By selecting erythritol which has the greatest phase change latent heat value among common phase change materials as an capsule core material, the microencapsulated phase change material prepared by the method of the invention has a phase change latent heat value of about 230J/g, which is substantially enhanced compared with the phase change latent heat values of microencapsulated phase change materials prepared by prior art.
Description
Technical field
The present invention relates to a kind of preparation method of functional composite material, specifically a kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials.
Background technology
Microencapsulated Phase Change Materials is stable solia particle under the normality that adopts microcapsulary that solid-liquid phase change material is coated with physics or chemical process with synthesized polymer material or mineral compound, this solia particle can absorb or discharge considerable latent heat of phase change in very narrow temperature range, there is more significant heat-accumulation temperature-adjustment function, by selecting, suitable capsule material can effectively improve the leakage of phase-changing energy storage material when solid-liquid phase change occurs, is separated, volumetric expansion, be corrosive, the problem such as poor heat stability.
The latent heat of phase change value of Microencapsulated Phase Change Materials is to estimate the important indicator of its performance.The latent heat of phase change value of Microencapsulated Phase Change Materials mainly determines by the latent heat of phase change value of core, and with the microcapsule rate (encapsulation rate) of phase change material, being shell in addition, how much content has relation.In theory, the ultimate value of microcapsule rate is 100%, and the latent heat of phase change value of Microencapsulated Phase Change Materials can approach the latent heat of phase change of phase change material.But in fact; the microcapsule rate can not surpass 80% usually; Microencapsulated Phase Change Materials is because the introducing of Shell Materials can cause the latent heat of phase change value significantly to descend usually, and report or its latent heat of phase change value of disclosed Microencapsulated Phase Change Materials are mostly lower than 100J/g at present.
Summary of the invention
For solving the lower problem of latent heat of phase change value of Microencapsulated Phase Change Materials, the invention provides a kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials.
The present invention solves the problems of the technologies described above the technical scheme of employing to be: a kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials comprises following steps:
1) prepare erythritol solution: the erythritol of getting by weight 8-15 part is dissolved in the deionized water of 16-30 part, add successively again the diethylenetriamine of 1-5 part, the Tween-80 of 0.01-1 part and the Span-80 of 0.05-2 part, make erythritol solution after stirring, standby;
2) isocyanic ester of 1-8 part is dissolved in the Witco 70 of 12-17 part, makes isocyanate solution, standby;
3) by the erythritol solution that makes in step 1 under the stirring velocity of 500-5000rpm, with the rate of addition of 10g/min, evenly be added drop-wise in the Witco 70 of 40-60 part, continue again to stir 0.5-1.5h after dropwising and make water-in-oil emulsion, standby;
4) by the isocyanate solution in step 2 under 50-60 ℃, the stirring velocity of 1000rpm, with the rate of addition of 0.5g/min, evenly be added drop-wise in the water-in-oil emulsion in step 3, standby;
5) make the mixture sustained reaction 1h under the condition of 60 ℃ in step 4, then filter, the solids distilled water wash after filtration, then it is dry to put into vacuum drying oven, obtains product.
Above-mentioned isocyanic ester can be monoisocyanates, vulcabond and polyisocyanates.
In the present invention, when each amount that participates in reaction is larger, be guaranteed efficiency and quality, can design a plurality of dropping points and stir spot, each rate of addition, stirring velocity that drips point all matches with above-mentioned rate of addition, stirring velocity.
Beneficial effect: the present invention does the capsule core by the erythritol of selecting latent heat of phase change value maximum in common phase change material, the Microencapsulated Phase Change Materials that uses the inventive method to prepare, its latent heat of phase change value is in the 230J/g left and right, and the latent heat of phase change value that has domestic Microencapsulated Phase Change Materials now is generally 110J/g, the product latent heat of phase change value of import is 151.6J/g, and the latent heat of phase change value of Microencapsulated Phase Change Materials prepared with prior art by the Microencapsulated Phase Change Materials that therefore uses present method to make is compared and had significant improvement.
Embodiment
Embodiment 1
A kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials comprises following steps:
1) prepare erythritol solution: the erythritol of getting 8g is dissolved in the deionized water of 22g, then adds successively the diethylenetriamine of 2g, the Tween-80 of 0.05g and the Span-80 of 0.1g, makes erythritol solution after stirring, standby;
2) tolylene diisocyanate of 1g is dissolved in the Witco 70 of 17g, makes tolylene diisocyanate solution, standby;
3) by the erythritol solution that makes in step 1 under the stirring velocity of 500rpm, with the rate of addition of 10g/min, evenly be added drop-wise in the Witco 70 of 50g, continue again to stir 0.5-1.5h after dropwising and make water-in-oil emulsion, standby;
4) by the tolylene diisocyanate solution in step 2 under 50 ℃, the stirring velocity of 1000rpm, with the rate of addition of 0.5g/min, evenly be added drop-wise in the water-in-oil emulsion in step 3, standby;
5) mixture in step 4 is warming up to 60 ℃, sustained reaction 1h, then filter, the solute distilled water wash after filtration, then put into vacuum drying oven, and at the temperature of 80 ℃, dry, obtain the product of particle diameter at the 30-50 micron.
The product obtained is used to the differential scanning calorimeter of U.S. PE company, the latent heat of phase change value that records this product under the condition of 10 ℃/min of temperature rise rate is 231.2J/g, far above the 151.6J/g of existing imported product and the 110.0J/g of homemade goods.
Embodiment 2
A kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials comprises following steps:
1) prepare erythritol solution: the erythritol of getting 11g is dissolved in the deionized water of 19g, then adds successively the diethylenetriamine of 2g, the Tween-80 of 0.05g and the Span-80 of 0.1g, makes erythritol solution after stirring, standby;
2) '-diphenylmethane diisocyanate of 5g is dissolved in the Witco 70 of 13g, makes '-diphenylmethane diisocyanate solution, standby;
3) by the erythritol solution that makes in step 1 under the stirring velocity of 1500rpm, with the rate of addition of 10g/min, evenly be added drop-wise in the Witco 70 of 50g, continue again to stir 0.5-1.5h after dropwising and make water-in-oil emulsion, standby;
4) by the '-diphenylmethane diisocyanate solution in step 2 under 50 ℃, the stirring velocity of 1000rpm, with the rate of addition of 0.5g/min, evenly be added drop-wise in the water-in-oil emulsion in step 3, standby;
5) mixture in step 4 is warming up to 60 ℃, sustained reaction 1h, then filter, the solute distilled water wash after filtration, then put into vacuum drying oven, and at the temperature of 80 ℃, dry, obtain the product of particle diameter at the 5-20 micron.
The product obtained is used to the differential scanning calorimeter of U.S. PE company, the latent heat of phase change value that records this product under the condition of 10 ℃/min of temperature rise rate is 237.1J/g, far above the 151.6J/g of existing imported product and the 110.0J/g of homemade goods.
Embodiment 3
A kind of preparation method of high latent heat of phase change value Microencapsulated Phase Change Materials comprises following steps:
1) prepare erythritol solution: the erythritol of getting 15g is dissolved in the deionized water of 13g, then adds successively the diethylenetriamine of 2g, the Tween-80 of 0.05g and the Span-80 of 0.1g, makes erythritol solution after stirring, standby;
2) triphenylmethane triisocyanate of 8g is dissolved in the Witco 70 of 12g, makes triphenylmethane triisocyanate solution, standby;
3) by the erythritol solution that makes in step 1 under the stirring velocity of 3000rpm, with the rate of addition of 10g/min, evenly be added drop-wise in the Witco 70 of 50g, continue again to stir 0.5-1.5h after dropwising and make water-in-oil emulsion, standby;
4) by the triphenylmethane triisocyanate solution in step 2 under 50 ℃, the stirring velocity of 1000rpm, with the rate of addition of 0.5g/min, evenly be added drop-wise in the water-in-oil emulsion in step 3, standby;
5) mixture in step 4 is warming up to 60 ℃, sustained reaction 1h, then filter, the solute distilled water wash after filtration, then put into vacuum drying oven, and at the temperature of 80 ℃, dry, obtain the product of particle diameter at the 0.1-5 micron.
The product obtained is used to the differential scanning calorimeter of U.S. PE company, the latent heat of phase change value that records this product under the condition of 10 ℃/min of temperature rise rate is 238.0J/g, far above the 151.6J/g of existing imported product and the 110.0J/g of homemade goods.
Claims (1)
1. the preparation method of one kind high latent heat of phase change value Microencapsulated Phase Change Materials, is characterized in that, comprises following steps:
1) prepare erythritol solution: the erythritol of getting by weight 8-15 part is dissolved in the deionized water of 16-30 part, add successively again the diethylenetriamine of 1-5 part, the Tween-80 of 0.01-1 part and the Span-80 of 0.05-2 part, make erythritol solution after stirring, standby;
2) isocyanic ester of 1-8 part is dissolved in the Witco 70 of 12-17 part, makes isocyanate solution, standby;
3) by the erythritol solution that makes in step 1 under the stirring velocity of 500-5000rpm, with the rate of addition of 10g/min, evenly be added drop-wise in the Witco 70 of 40-60 part, continue again to stir 0.5-1.5h after dropwising and make water-in-oil emulsion, standby;
4) by the isocyanate solution in step 2 under 50-60 ℃, the stirring velocity of 1000rpm, with the rate of addition of 0.5g/min, evenly be added drop-wise in the water-in-oil emulsion in step 3, standby;
5) make the mixture sustained reaction 1h under the condition of 60 ℃ in step 4, then filter, the solids distilled water wash after filtration, then it is dry to put into vacuum drying oven, obtains product.
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| CN103804558A (en) * | 2012-11-15 | 2014-05-21 | 上海华明高技术（集团）有限公司 | Nano phase change material emulsion wide in temperature change range and preparation method thereof |
| CN105980511B (en) * | 2014-02-14 | 2020-06-02 | 日立化成株式会社 | Sugar alcohol microcapsule, slurry, and resin molded article |
| CN104610921A (en) * | 2014-12-26 | 2015-05-13 | 上海维凯光电新材料有限公司 | PA66/xylitol microcapsule heat storage material and preparation method thereof |
| CN104830281B (en) * | 2015-05-07 | 2017-12-05 | 长沙理工大学 | A kind of medium temperature composite shape-setting phase-change heat-storage material and preparation method thereof |
| CN105944636B (en) * | 2016-04-27 | 2018-05-04 | 扬州大学 | The method that original position-micro emulsion interface copolymerization method prepares potassium peroxydisulfate microcapsules |
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Non-Patent Citations (4)
| Title |
|---|
| 《Microencapsulation of a cooling agent by interfacial polymerization: Influence of the parameters of encapsulation on poly(urethane–urea) microparticles characteristics》;F.Salaun et al.;《Journal of Membrane Science》;20101130;第370卷(第1-2期);第23-33页 * |
| 《Thermophysical and heat transfer properties of phase change material candidate for waste heat transportation system》;Akihide Kaizawa et al.;《Heat Mass Transfer》;20070714;第44卷(第7期);第763-769页 * |
| Akihide Kaizawa et al..《Thermophysical and heat transfer properties of phase change material candidate for waste heat transportation system》.《Heat Mass Transfer》.2007,第44卷(第7期), |
| F.Salaun et al..《Microencapsulation of a cooling agent by interfacial polymerization: Influence of the parameters of encapsulation on poly(urethane–urea) microparticles characteristics》.《Journal of Membrane Science》.2010,第370卷(第1-2期), |
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