CN102676123A - Microcapsule preparation method of phase change material - Google Patents
Microcapsule preparation method of phase change material Download PDFInfo
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- CN102676123A CN102676123A CN2012101050564A CN201210105056A CN102676123A CN 102676123 A CN102676123 A CN 102676123A CN 2012101050564 A CN2012101050564 A CN 2012101050564A CN 201210105056 A CN201210105056 A CN 201210105056A CN 102676123 A CN102676123 A CN 102676123A
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Abstract
The invention discloses a microcapsule preparation method of a phase change material. The defects of containing of methanol, poor environment friendliness, easiness in cracking in a capsule energy storing process and poor energy storing effect exist in a phase change microcapsule prepared with the conventional method. The method comprises the following steps of: emulsifying a phase change material into a nuclear phase by adopting an interface polymerization method, wherein the phase change material accounts for 20-60 percent; preparing styryl and acrylate monomers into a shell phase; and mixing the two phases, polymerizing at the temperature of 80-160 DEG C, reacting for 2-6 hours, preserving heat for 1-4 hours, cooling and drying to obtain a phase change microcapsule. Formaldehyde is not required to be added in a preparation process, and a production process is environment-friendly; after a capsule is prepared, the capsule wall coating property is high, and reaction time is shortened; the method is low in preparation cost, has a simple and convenient process and contributes to industrial production; and the obtained product can be widely applied in the fields of building energy storage, energy saving, consumption reduction, spinning and the like.
Description
Technical field
What the present invention relates to is a kind of coating technology of phase change material, specifically refers to a kind of preparation method of microcapsules of storing energy through phase change, belongs to new material technology field.
Background technology
Phase change material can absorb in phase transition process or emit a large amount of latent heat, is a kind of energy-saving material that is widely used in heat storage and domain of control temperature.Come to light the sixties in 20th century, developed rapidly in American-European countries after the seventies.Be widely used in fields such as HVAC, building energy conservation, sun power utilization, clothes insulation, be significant aspect the energy-conservation energy-saving and emission-reduction.
Phase-change microcapsule is exactly to use microcapsulary at the surperficial composite phase-change material with nucleocapsid structure that coats the film of one deck stable performance and constitute of solid-liquid phase change particles of material; Can improve the stability of solid-liquid phase change material behind the micro encapsulation greatly; Reduce the reaction of phase change material and external environment, and can increase heat exchange area.Therefore the micro encapsulation of phase change material more and more receives researchist's concern.
The microcapsule that worked out at present have multiple preparation method, and people such as Zhang Shengxiang are at document " Thermal stability and permeability of microencapsulated n-octadecane and cyclohexane.Ther mochinica Acta.2005; 429 (1): 25-29 " studied in and used situ aggregation method to be capsule-core, melamine formaldehyde resin microcapsule as the wall material with Octadecane.Is that capsule-core, melamine formaldehyde resin are in the microcapsule preparation of wall material with the Octadecane, pH value, thermal treatment temp are bigger to capsular stability influence, and the add-on of bicyclohexane has bigger influence to the depression probability of microcapsule.People such as Wang Lixin document " development of phase-change thermal storage microcapsule. polymer material science and engineering .2005,21 (1): 256-259 " in to adopt situ aggregation method to coat a kind of transformation temperature with melmac be that 24 ℃, latent heat of phase change are the composite phase-change material of 225.5j/g.Experimental result shows: phase-change microcapsule is sphere, particle diameter 5.5 μ m; The smooth densification of capsule surface does not have any leakage; Phase-change thermal storage does not influence the transformation temperature and the heat of phase transformation of phase change material.Yet said process prepares microcapsule has used formaldehyde, and formaldehyde does not solve the pollution of environment and the big problem of harm of human body, and transformation efficiency is low, and preparation cost is big.
Application number is 200510024707.7 one Chinese patent application, discloses a kind of technology that adopts the synthetic phase-change microcapsule of method of emulsion hud polymerization.This technology is that the organic phase change material in the time of 10-90 ℃ is a core; With vinyl and bi-vinyl type free base monomer is the outer cover polymer source; With water is polymerisation medium, is emulsifying agent with nonionic and AS, and the redox couple that persulphate, perphosphate, perborate, hydrogen peroxide or these superoxide and reductive agent are formed is an initiator; Under 0-100 ℃ temperature, carry out emulsion hud polymerization parcel, make this phase-change microcapsule.Yet the used emulsifying agent function singleness of emulsion polymerization prepared phase-change microcapsule is unfavorable for the formation of microcapsule, thereby has caused lower encapsulated output capacity.The above-mentioned technology that discloses all exists certain deficiency, and this is just pointing out the technology of preparing at microcapsules of storing energy through phase change also to need technical progress, goes to improve these deficiencies, therefore further investigation, and overcoming existing deficiency is meaning of the present invention.
Summary of the invention
The object of the invention just provides a kind of preparation method of microcapsules of storing energy through phase change, overcomes the methyl alcohol that contains that the phase-change microcapsule of existing method preparation exists in the preparation process, not environmental protection, and the capsule thermal energy storage process is prone to break, the deficiency that the energy storage effect is not high.
For realizing the foregoing invention purpose, the present invention has taked such technical scheme: a kind of preparation method of microcapsules of storing energy through phase change, and concrete steps are:
(1) preparation glue nuclear phase: with 1: 1-5: the weight ratio of 0.25-0.5; Get phase change material and mix with emulsifying agent with water, use homogenate shears high speed dispersion, rate of dispersion is 3000-8000r/min; It is not stratified that milkiness leaves standstill in 24 hours night, and it is subsequent use to obtain the glue nuclear phase;
(2) preparation shell facies: with styryl, acrylic ester monomer according to 3-5: 1 weight ratio is mixed; The mixed solution of the water that to add hundred parts of content of weight again are 15-25%, emulsifying agent, catalyzer, initiator; Be mixed together and stir; It is subsequent use to obtain shell facies, and wherein the weight ratio of water and monomer and catalyzer and initiator is 1 in the mixed solution: 2-4: 0.1-0.2: 0.05-0.1;
(3) above-mentioned glue nuclear phase is placed container,, and keep constant temperature 80-90 ℃ with the slowly at the uniform velocity stirring of speed of 200-500r/min; Speed with the 1-4 ml/min splashes into shell facies, and wherein the weight ratio of shell facies and glue nuclear phase adding is 1-5: 1; Reacted 2-6 hour down at temperature 80-160 ℃, be incubated 1-4 hour, when being cooled to 50 ℃; Add ammoniacal liquor and be adjusted to pH 7-9, in 50-60 ℃ vacuum drying box, dry, obtain phase-change microcapsule to constant weight.
Said phase change material refers to a kind of or any mixture in n-hexadecane, NSC 62789, Octadecane, n-docosane, positive octacosane, capric acid, LAURIC ACID 99 MIN, tetradecanoic acid, Palmiticacid, Triple Pressed Stearic Acid or the NSC 6366, and said phase change material all is commercially available industrial commodity;
Said acrylic ester monomer refers to a kind of or any mixture in TEB 3K, Bing Xisuandingzhi, Isooctyl acrylate monomer, vinylformic acid or the acrylic acid amides, and above-mentioned materials all is commercially available industrial commodity;
Described emulsifying agent refers to a kind of or any mixture in this dish-60, Tween-60, sodium lauryl sulphate, polyoxyethylene carboxylate or the phenolic ether sulfosuccinic ester disodium, and above-mentioned materials all is commercially available industrial commodity;
Said catalyzer refers to a kind of or any mixture in ammonium persulphate, ferrous sulfate, Sodium Persulfate, Potassium Persulphate or the Sodium Pyrosulfite, and above-mentioned materials all is commercially available industrial commodity;
Said initiator refers to a kind of or any mixture in ammonium sulfate, ferrous sulfate, Sodium Persulfate, the Potassium Persulphate, and above-mentioned materials all is commercially available industrial commodity.
Take the present invention of above-mentioned measure, compared with prior art, have following advantage: 1) the present invention prepares process and need not add formaldehyde, environmental protection in the process of producing; 2) the present invention adopts situ aggregation method, nucleocapsid is divided to come mutually carry out prefabricatedly, helps the stable of shell facies and nuclear phase, and after preparing capsule, the cyst wall covering property is good, and phase change material spills probability to be reduced; 3) cyst material good toughness when the cold and hot expansion of kernel is shunk, is alleviated the pressure that phase change material produces, and cyst wall does not break, and guarantees that the heat storage capacity of microcapsule does not reduce; 4) reaction times shortens, and preparation cost reduces, and can aspect building energy conservation, enlarge promoted extension.Preparation cost of the present invention is low, and technology is easy, helps suitability for industrialized production; Products obtained therefrom can be widely used in building fields such as energy storage, energy-saving and cost-reducing, weaving.
Embodiment
Embodiment 1
(1) preparation nuclear phase: get n-hexadecane 33g, Span-80 8.3g mixes the back and adds reaction kettle, with 500 rev/mins speed, stirs and be warmed to 55 ℃ at a slow speed; Splash into deionized water 133g then, Tween-60 0.83g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 4500r/min, stirs 5min, disperses to accomplish subsequent use;
(2) preparation shell facies: remove ionized water 78g, vinylbenzene 22g, TEB 3K 48g, emulsifying agent phenolic ether sulfosuccinic ester disodium 5g mixes back speed with 350 rev/mins in reaction kettle and stirs and be warmed up to 60 ℃ at a slow speed; Getting ammonium persulphate 0.15g and 4.1g deionized water, to be mixed with into initiator subsequent use; Getting Sodium Pyrosulfite 0.05g and 15g deionized water, to be mixed with into catalyzer subsequent use.
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 4 hours, is incubated 1 hour afterwards; The ammoniacal liquor that adds 2.1g when being cooled to below 50 ℃ then; In 50 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Embodiment 2
(1) preparation nuclear phase: get n-capric acid 6g, Span-80 1.5g mixes the back and adds reaction kettle, with 550 rev/mins speed, stirs and be warmed to 55 ℃ at a slow speed; Drip deionized water 24g then, sodium lauryl sulphate 0.15g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 4500r/min, stirs 5min, disperses to accomplish subsequent use;
(2) preparation shell facies: remove ionized water 36g, vinylbenzene 11g, Isooctyl acrylate monomer 24g, 60 ℃ are stirred and be warmed up in emulsifying agent phenolic ether sulfosuccinic ester disodium 2.5g mixing back with 300 rev/mins speed, at a slow speed in reaction kettle; Getting ferrous sulfate 0.07g and 2.0g deionized water, to be mixed with into initiator subsequent use; Getting Sodium Pyrosulfite 0.03g and 15g deionized water, to be mixed with into catalyzer subsequent use;
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 4 hours, back insulation 1 hour; The ammoniacal liquor that adds 1.5g when being cooled to below 50 ℃ then; In 50 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Embodiment 3
(1) preparation nuclear phase: n-docosane is respectively got 5g with positive octacosane, and Span-80 2.5g mixes the back and adds reaction kettle, with 450 rev/mins speed, stirs and be warmed to 55 ℃ at a slow speed; Drip deionized water 40g then, Tween-60 0.4g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 6000r/min, stirs 5min, disperses to accomplish subsequent use.
(2) preparation shell facies: remove ionized water 120g, vinylbenzene 30g, acrylic acid amides 65g, emulsifying agent polyoxyethylene carboxylate 6g, 60 ℃ are stirred and be warmed up in the mixing back with 300 rev/mins speed, at a slow speed in reaction kettle; Getting Potassium Persulphate 0.21g and 5.7g deionized water, to be mixed with into initiator for use; Getting Sodium Pyrosulfite 0.08g and 24g deionized water, to be mixed with into catalyzer subsequent use;
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 3 hours, back insulation 1 hour; The ammoniacal liquor that adds 3.1g when being cooled to below 50 ℃ then; In 60 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Embodiment 4
(1) preparation nuclear phase: get Octadecane 10g, sodium lauryl sulphate 2.5g mixes the back and adds reaction kettle, stirs and be warmed to 55 ℃ at a slow speed with 550 rev/mins speed; Drip deionized water 40g then, Tween-60 0.25g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 6500r/min, stirs 5min, disperses to accomplish for use;
(2) preparation shell facies: remove ionized water 105g, vinylbenzene 33g, Bing Xisuandingzhi 72g, emulsifying agent phenolic ether sulfosuccinic ester disodium 7.5g, 60 ℃ are stirred and be warmed up in the mixing back with 300 rev/mins speed, at a slow speed in reaction kettle; Getting Sodium Persulfate 0.25g and 6.1g deionized water, to be mixed with into initiator subsequent use; Getting Potassium Persulphate 0.07g and 22g deionized water, to be mixed with into catalyzer subsequent use;
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 2 hours, back insulation 1 hour; The ammoniacal liquor that adds 3.1g when being cooled to below 50 ℃ then; In 53 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Embodiment 5
(1) preparation nuclear phase: get n-teradecanoic acid 9g, Span-80 2.3 mixes the back and adds reaction kettle, with 450 rev/mins speed, stirs and be warmed to 55 ℃ at a slow speed; Drip deionized water 36g then, Span-80 0.23g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 5500r/min, stirs 5min, disperses to accomplish subsequent use;
(2) preparation shell facies: remove ionized water 88g, vinylbenzene 28g, TEB 3K 62g, emulsifying agent phenolic ether sulfosuccinic ester disodium 7g, 60 ℃ are stirred and be warmed up in the mixing back with 300 rev/mins speed, at a slow speed in reaction kettle; Getting Sodium Pyrosulfite 0.20g and 5.3g deionized water, to be mixed with into initiator for use; Getting ammonium persulphate 0.06g and 20g deionized water, to be mixed with into catalyzer subsequent use;
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 5 hours, back insulation 2 hours; The ammoniacal liquor that adds 2.8g when being cooled to below 50 ℃ then; In 55 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Embodiment 6
(1) preparation nuclear phase: get LAURIC ACID 99 MIN 90g, Tween-60 22g mixes the back and adds reaction kettle, stirs and be warmed to 55 ℃ at a slow speed with 450 rev/mins speed; Drip deionized water 360g then, Tween-60 2.2g stirs 20min at a slow speed under the constant temperature, improves stirring velocity afterwards to 5500r/min, stirs 5min, disperses to accomplish for use;
(2) preparation shell facies: remove ionized water 140g, vinylbenzene 91g, vinylformic acid 198g, emulsifying agent phenolic ether sulfosuccinic ester disodium 19.3g mixes back speed with 300 rev/mins in reaction kettle and stirs and be warmed up to 60 ℃ at a slow speed; Getting ammonium persulphate 0.6g and 16.8g deionized water, to be mixed with into initiator for use; Getting ferrous sulfate 0.19g and 60.5g deionized water, to be mixed with into catalyzer subsequent use;
(3) shell facies is added drop-wise in the nuclear phase under 80 ℃ of constant temperature, and adds above-mentioned initiator, catalyzer simultaneously, the dropping time is controlled at 2-3h, is added dropwise to complete continued constant temperature stirring reaction 6 hours, back insulation 2 hours; The ammoniacal liquor that adds 3.1g when being cooled to below 50 ℃ then; In 56 ℃ vacuum drying box, dry at last, obtain phase-change microcapsule to constant weight.
Claims (1)
1. the preparation method of a microcapsules of storing energy through phase change is characterized in that said method is:
(1) preparation glue nuclear phase: with 1: 1-5: the weight ratio of 0.25-0.5; Get phase change material and mix with emulsifying agent with water, use homogenate shears high speed dispersion, rate of dispersion is 3000-8000r/min; It is not stratified that milkiness leaves standstill in 24 hours night, and it is subsequent use to obtain the glue nuclear phase;
(2) preparation shell facies: with styryl, acrylic ester monomer according to 3-5: 1 weight ratio is mixed; The mixed solution of the water that to add hundred parts of content of weight again are 15-25%, emulsifying agent, catalyzer, initiator; Be mixed together and stir; It is subsequent use to obtain shell facies, and wherein the weight ratio of water and monomer and catalyzer and initiator is 1 in the mixed solution: 2-4: 0.1-0.2: 0.05-0.1;
(3) above-mentioned glue nuclear phase is placed container,, and keep constant temperature 80-90 ℃ with the slowly at the uniform velocity stirring of speed of 200-500r/min; Speed with the 1-4 ml/min splashes into shell facies, and wherein the weight ratio of shell facies and glue nuclear phase adding is 1-5: 1; Reacted 2-6 hour down at temperature 80-160 ℃, be incubated 1-4 hour, when being cooled to 50 ℃; Add ammoniacal liquor and be adjusted to pH 7-9, in 50-60 ℃ vacuum drying box, dry, obtain phase-change microcapsule to constant weight;
Said phase change material refers to a kind of or any mixture in n-hexadecane, NSC 62789, Octadecane, n-docosane, positive octacosane, capric acid, LAURIC ACID 99 MIN, tetradecanoic acid, Palmiticacid, Triple Pressed Stearic Acid or the NSC 6366;
Said acrylic ester monomer refers to a kind of or any mixture in TEB 3K, Bing Xisuandingzhi, Isooctyl acrylate monomer, vinylformic acid or the acrylic acid amides;
Described emulsifying agent refers to a kind of or any mixture in this dish-60, Tween-60, sodium lauryl sulphate, polyoxyethylene carboxylate or the phenolic ether sulfosuccinic ester disodium;
Said catalyzer refers to a kind of or any mixture in ammonium persulphate, ferrous sulfate, Sodium Persulfate, Potassium Persulphate or the Sodium Pyrosulfite;
Said initiator refers to a kind of or any mixture in ammonium sulfate, ferrous sulfate, Sodium Persulfate, the Potassium Persulphate.
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| CN104031612A (en) * | 2013-03-07 | 2014-09-10 | 中国科学院化学研究所 | Phase change energy storage microcapsule and preparation method thereof |
| CN103805142A (en) * | 2013-12-30 | 2014-05-21 | 清华大学深圳研究生院 | Silicon nitride-modified phase-change and energy-storage microcapsule and preparation method thereof |
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| CN104610923A (en) * | 2015-01-13 | 2015-05-13 | 福建建工建材科技开发有限公司 | Phase change energy storage material for reflective heat-insulating coating |
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| CN107062971B (en) * | 2017-03-27 | 2019-02-19 | 上海交通大学 | A kind of efficient phase-change energy storage packaging body |
| CN107062971A (en) * | 2017-03-27 | 2017-08-18 | 上海交通大学 | A kind of efficient phase-change energy storage packaging body |
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| CN110711545A (en) * | 2019-11-18 | 2020-01-21 | 深圳先进技术研究院 | Phase change energy storage microcapsule with organic silazane polymer resin as shell material and preparation method thereof |
| CN110711545B (en) * | 2019-11-18 | 2021-03-16 | 深圳先进技术研究院 | Phase change energy storage microcapsule with organic silazane polymer resin as shell material and preparation method thereof |
| CN111574934A (en) * | 2020-05-19 | 2020-08-25 | 常州百佳年代薄膜科技股份有限公司 | Nano heat-conducting adhesive film, microcapsule, preparation method of microcapsule, photovoltaic module and detection method |
| CN111944371A (en) * | 2020-08-10 | 2020-11-17 | 江苏可米新材料科技有限公司 | Self-repairing temperature-adjustable functional coating and preparation method thereof |
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Application publication date: 20120919 |