CN104877642A - Phase-change microcapsule composition material and preparation method thereof - Google Patents
Phase-change microcapsule composition material and preparation method thereof Download PDFInfo
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- CN104877642A CN104877642A CN201510336603.3A CN201510336603A CN104877642A CN 104877642 A CN104877642 A CN 104877642A CN 201510336603 A CN201510336603 A CN 201510336603A CN 104877642 A CN104877642 A CN 104877642A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
Abstract
The invention discloses a phase-change microcapsule composition material and a preparation method thereof. The material is a microcapsule of a core-wall structure and consists of a core material (1) and a wall material (2), wherein the core material is one or some of phase-change materials, namely, MgCl2.6H2O and Mg(NO3)2.2H2O and D-mannitol; the wall material is one or some of polystyrene, polymethyl methacrylate, urea resin and polyacrylonitrile or a composition material of the high-molecular polymer above and graphene; the core material (1) is 35 to 85% by mass based on the total mass of the microcapsule composition material, and the wall material (2) is 15 to 65% by mass based on the total mass of the microcapsule composition material; the phase-change point of the prepared phase-change microcapsule composition material is between 100 to 200 DEG C, and the particle size is 3 to 4 microns. The prepared phase-change microcapsule composition material is good in wrapping rate, high in sealing performance, high in phase-change latent heat, small in raw material cost, and simple in preparation process.
Description
Technical field
The present invention relates to a kind of phase-change microcapsule matrix material, and provide the preparation method of this matrix material, belong to energy storage material field.
Background technology
The energy is the basis that the mankind depend on for existence.At present along with the high speed development of global industry, global energy is worsening shortages also, and the exhaustion crisis of the energy and problem of environmental pollution are more and more subject to people and pay close attention to, and improves energy use efficiency and develops the important topic that renewable energy source is facing mankind.At present, because phase change material can utilize the heat absorption and release effect of material in phase transition process effectively to carry out thermal energy storage and temperature adjusting, be widely used in alleviating energy crisis, raising energy utilization rate etc.Utilizing the latent heat of phase change of phase change material to realize storage and the utilization of energy, improve energy use efficiency and exploitation renewable energy source, is a new focus in energy science and material science in recent years.Phase-change heat-storage material all will show wide application prospect in engineering lagging material, energy-conservation, energy storage cooker, aerospace material etc.Along with nanometer technique further develops, the preparation of composite phase-change material combined with nanometer technique, preparing efficient micro-/ nano composite phase-change material is just becoming the very active research direction of of heat-storage technology field.
Microcapsulary is a kind of method that film forming material is overmolding to solid or liquid the particulate with nucleocapsid structure, and the research of microencapsulated phase change material will be that microcapsulary is applied to the new research field formed in phase change material.This solia particle can absorb or discharge objective latent heat of phase change in little temperature range.The particle diameter of microcapsule is usually at 0.1 ~ 1000 μm, and outer casing thickness is not at 0.01 ~ 10 μm etc.Microencapsulated phase change material overcomes the application limitation of phase change material technically, improves the service efficiency of phase change material, has widened the Application Areas of phase change material, has had broad application prospects.
Be core as Chinese patent CN200610066248.3 discloses a kind of with paraffin, the phase-change microcapsule material being cyst material with tolylene diisocyanate and urea-formaldehyde resin bi-material, the transformation temperature of this material is from 0 DEG C ~ 70 DEG C.Chinese patent CN201410035306.0 discloses a kind of lauryl alcohol/melamine-forresinhyde resinhyde microcapsule phase-change material, and this material is with lauryl alcohol emulsion for core, and melamine formaldehyde resin is wall.These phase-change microcapsule materials all cannot meet the demand of the middle-temperature section application of 100 ~ 200 DEG C, and therefore in exploitation, warm phase-change microcapsule material has great importance and vast potential for future development.
Summary of the invention
The object of this invention is to provide a kind of phase-change microcapsule matrix material, it is characterized in that phase-change microcapsule matrix material is made up of core (1) and wall material (2), core (1) is phase change material, the mass percent that core (1) accounts for microcapsule composite material total amount is 35% ~ 85%, wall material (2) is high molecular polymer or high molecular polymer-graphene composite material, and the mass percent that wall material (2) accounts for microcapsule composite material total amount is 15% ~ 65%.Core is MgCl
26H
2o, Mg (NO
3)
22H
2one or more in O and PEARLITOL 25C, wall material is monomer is the polymkeric substance or above-mentioned polymkeric substance and graphene composite material that in vinylbenzene, methyl methacrylate, formaldehyde, urea and vinyl cyanide, one or more are polymerized.The phase-change microcapsule matrix material particle diameter of gained is at 3 ~ 4 μm.
Phase-change microcapsule matrix material is realized by following steps:
(1) method one:
A. weighing core materials and deionized water are mixed to get core saturated solution;
B. in the saturated solution that A is obtained, add emulsifying agent, emulsification 40 ~ 60min in clarifixator, with magnetic stirrer dispersion 20 ~ 60min in the water-bath of 50 ~ 60 DEG C, obtain homogeneous latex emulsion (a);
C. by the monomer of wall material/polymer, to be dissolved in deionized water and to regulate pH to be 8 ~ 8.6, constant temperature at 70 ~ 75 DEG C, reacting 1 ~ 3h under 450 ~ 600rpm rotating speed and obtain clear prepolymer liquid solution (b);
D. homogeneous latex emulsion (a) is slowly dropped in clear prepolymer liquid solution (b), regulate pH to be 2.5 ~ 3.5, at 70 ~ 75 DEG C, after 600 ~ 800rpm stirs 2.5 ~ 3.5h, with acetone and deionized water wash drying, vacuum filtration, obtains phase-change microcapsule matrix material.
(2) method two
A. weighing core materials, emulsifying agent, organic solvent, disperses 40 ~ 60min, obtains homogeneous latex emulsion in ultrasonic wave;
B. polymer monomer, Graphene and initiator are slowly added drop-wise in above-mentioned homogeneous latex emulsion, under 50 DEG C ~ 70 DEG C waters bath with thermostatic control, with 600 ~ 900rpm stir speed (S.S.), after reaction 9 ~ 12h, vacuum filtration, spends acetone and deionized water wash is dry, obtains phase-change microcapsule matrix material.
Initiator described in aforesaid method is the one in Diisopropyl azodicarboxylate, dibenzoyl peroxide, ammonium persulphate, and emulsifying agent is the one in Sodium dodecylbenzene sulfonate, SPAN-80, and organic solvent is one or both in normal hexane, toluene.
Advantage of the present invention:
Phase-change microcapsule matrix material transformation temperature prepared by the present invention is between 100 ~ 200 DEG C, and clad ratio is good, good airproof performance, and latent heat of phase change is high, and raw materials cost is lower, and preparation technology is simple.
Embodiment
In conjunction with case study on implementation, the present invention is described in further details, but scope is not limited to described content.
Embodiment 1:
Take the MgCl of 3.5g
26H
2o, is made into saturated solution with deionized water, adds 0.45g Sodium dodecylbenzene sulfonate, fully emulsified 40min in clarifixator, then it is used magnetic stirring apparatus emulsification 20min in 50 DEG C of waters bath with thermostatic control, obtains homogeneous latex emulsion (a); Taking 2.8g urea and 3.7g dissolve formaldehyde in deionized water regulates pH to be 8.6.At 70 DEG C, under the rotating speed of 450rpm, stir 1h, obtain transparent urea resin prepolymer solution (b); Emulsion (a) is slowly dropped in prepolymer solution (b), regulates pH to be 3, at 70 DEG C, 2.5h is reacted, vacuum filtration under the rotating speed of 600rpm, and with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 2:
Take 6g MgCl
26H
2o, is made into saturated solution with ionized water, adds 0.6g Sodium dodecylbenzene sulfonate, fully emulsified 50min in clarifixator, then it is used magnetic stirring apparatus emulsification 40min in 55 DEG C of waters bath with thermostatic control, obtains homogeneous latex emulsion (a); 1.7g urea and 2.3g dissolve formaldehyde are in deionized water and regulate pH to be 8.6; At 73 DEG C, under the rotating speed of 500rpm, stir 2.5h, obtain transparent urea resin prepolymer solution (b); Emulsion (a) is slowly dropped in prepolymer solution (b), regulates pH to be 3, at 72 DEG C, 3h is reacted, vacuum filtration under the rotating speed of 800rpm, and with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 3:
Take 8.5g Mg (NO3)
22H
2o, is made into saturated solution with ionized water, adds 0.8g Sodium dodecylbenzene sulfonate, fully emulsified 60min in clarifixator, then it is used magnetic stirring apparatus emulsification 60min in 60 DEG C of waters bath with thermostatic control, obtains homogeneous latex emulsion (a); 0.64g urea and 0.86g dissolve formaldehyde are in deionized water and regulate pH to be 8.6; At 75 DEG C, under the rotating speed of 550rpm, stir 3h, obtain transparent urea resin prepolymer solution (b); Emulsion (a) is slowly dropped in prepolymer solution (b), regulates pH to be 3.5, at 74 DEG C, 3.5h is reacted, vacuum filtration under the rotating speed of 700rpm, and with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 4:
Take 8.5g Mg (NO3)
22H
2o and certain deionized water mix, then under the water bath with thermostatic control of 40 DEG C, 0.8g Sodium dodecylbenzene sulfonate is added, fully emulsified 60min in clarifixator, then uses magnetic stirring apparatus emulsification 20min by it, obtains homogeneous latex emulsion (a) in 55 DEG C of waters bath with thermostatic control; 0.64g urea and 0.86g dissolve formaldehyde are in deionized water and regulate pH to be 8.6; At 75 DEG C, under the rotating speed of 600rpm, stir 3h, obtain transparent urea resin prepolymer solution (b); Emulsion (a) is slowly dropped in prepolymer solution (b), regulates pH to be 2.5, at 70 DEG C, 3h is reacted, vacuum filtration under the rotating speed of 800rpm, and with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 5:
Take 4g Mg (NO3)
22H
2o, 0.4g SPAN-80 and 40ml normal hexane, disperses 40min by ultrasonic wave, obtains homogeneous latex emulsion; 0.12g Diisopropyl azodicarboxylate is joined in above-mentioned emulsion, and 6g acrylonitrile monemer is slowly dropped in emulsion, 50 DEG C of water-baths, 9h is reacted, vacuum filtration under the rotating speed of 800rpm, and dry with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 6:
Take 6g PEARLITOL 25C, 0.45g SPAN-80 and 40ml normal hexane, disperse 50min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g dibenzoyl peroxide is joined in above-mentioned emulsion, and 4g acrylonitrile monemer is slowly dropped in emulsion, 50 DEG C of water-baths, 10h is reacted, vacuum filtration under the rotating speed of 900rpm, and dry with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 7:
Take 6g Mg (NO3)
22H
2o, 0.45g Sodium dodecylbenzene sulfonate and 40ml toluene, disperse 45min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g ammonium persulphate is joined in above-mentioned emulsion, and 4g styrene monomer is slowly dropped in emulsion, 60 DEG C of water-baths, 11h is reacted, vacuum filtration under the rotating speed of 900rpm, and dry with acetone and deionized water wash, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 8:
Take 8g MgCl
22H
2o, 0.5g Sodium dodecylbenzene sulfonate and 40ml normal hexane, disperse 55min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g ammonium persulphate is joined in above-mentioned emulsion, and 2g methyl methacrylate monomer is slowly dropped in emulsion, 70 DEG C of water-baths, 12h is reacted under the rotating speed of 800rpm, vacuum filtration, and with acetone and deionized water wash drying, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 9:
Take 6g Mg (NO3)
22H
2o, 0.2g PEARLITOL 25C, 0.45g Sodium dodecylbenzene sulfonate and 40ml normal hexane, disperse 60min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g ammonium persulphate is joined in above-mentioned emulsion, and 4g methyl methacrylate monomer is slowly dropped in emulsion, 70 DEG C of water-baths, 12h is reacted under the rotating speed of 900rpm, vacuum filtration, and with acetone and deionized water wash drying, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 10:
Take 6g Mg (NO3)
22H
2o, 0.45g Sodium dodecylbenzene sulfonate and 40ml normal hexane, disperse 45min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g ammonium persulphate is joined in above-mentioned emulsion, and 3.8g styrene monomer slowly to be dropped in emulsion and to add 0.2g graphene powder, 60 DEG C of water-baths, 11h is reacted under the rotating speed of 900rpm, vacuum filtration, and with acetone and deionized water wash drying, obtain pressed powder, be phase-change microcapsule matrix material.
Embodiment 11:
Take 8g Mg (NO3)
22H
2o, 0.45g Sodium dodecylbenzene sulfonate and 40ml toluene, disperse 60min by ultrasonic wave, obtain homogeneous latex emulsion; 0.12g ammonium persulphate is joined in above-mentioned emulsion, and 1.9g methyl methacrylate monomer slowly to be dropped in emulsion and to add 0.1g Graphene, 60 DEG C of water-baths, 11h is reacted under the rotating speed of 900rpm, vacuum filtration, and with acetone and deionized water wash drying, obtain pressed powder, be phase-change microcapsule matrix material.
Claims (4)
1. a phase-change microcapsule matrix material, be made up of core (1) and wall material (2), described core (1) is phase change material, the mass percent that core (1) accounts for microcapsule composite material total amount is 35% ~ 85%, described wall material (2) is high molecular polymer or high molecular polymer-graphene composite material, and the mass percent that wall material (2) accounts for microcapsule composite material total amount is 15% ~ 65%.
2. the phase-change microcapsule matrix material according to claims 1, is characterized in that described core is MgCl
26H
2o, Mg (NO
3)
22H
2one or more in O and PEARLITOL 25C, wall material is monomer is the polymkeric substance or above-mentioned polymkeric substance and graphene composite material that in vinylbenzene, methyl methacrylate, formaldehyde, urea, vinyl cyanide, one or more are polymerized.
3. the preparation method of a kind of phase-change microcapsule matrix material according to claim 1, tests by following steps:
(1) method one:
A. weighing core materials and deionized water are mixed to get core saturated solution;
B. in the saturated solution that A is obtained, add emulsifying agent, emulsification 40 ~ 60min in clarifixator, with magnetic stirrer dispersion 20 ~ 60min in the water-bath of 50 ~ 60 DEG C, obtain homogeneous latex emulsion (a);
C. by the monomer of wall material/polymer, to be dissolved in deionized water and to regulate pH to be 8 ~ 8.6, constant temperature at 70 ~ 75 DEG C, reacting 1 ~ 3h under 450 ~ 600rpm rotating speed and obtain clear prepolymer liquid solution (b);
D. homogeneous latex emulsion (a) is slowly dropped in clear prepolymer liquid solution (b), regulate pH to be 2.5 ~ 3.5, at 70 ~ 75 DEG C, after 600 ~ 800rpm stirs 2.5 ~ 3.5h, with acetone and deionized water wash drying, vacuum filtration, obtains phase-change microcapsule matrix material.
(2) method two
A. weighing core materials, emulsifying agent, organic solvent, disperses 40 ~ 60min, obtains homogeneous latex emulsion in ultrasonic wave;
B. polymer monomer, Graphene and initiator are slowly added drop-wise in above-mentioned homogeneous latex emulsion, under 50 DEG C ~ 70 DEG C waters bath with thermostatic control, with 600 ~ 900rpm stir speed (S.S.), after reaction 9 ~ 12h, vacuum filtration, spends acetone and deionized water wash is dry, obtains phase-change microcapsule matrix material.
4. the preparation method of a kind of phase-change microcapsule matrix material according to claims 3, it is characterized in that described initiator is the one in Diisopropyl azodicarboxylate, dibenzoyl peroxide, ammonium persulphate, emulsifying agent is the one in Sodium dodecylbenzene sulfonate, SPAN-80, and organic solvent is one or both in normal hexane, toluene.
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|---|---|---|---|---|
| CN106350018A (en) * | 2016-07-29 | 2017-01-25 | 上海应用技术学院 | Water-free microwave heating energy-storing microcapsule with hot compress function and preparation method |
| CN106732222A (en) * | 2017-03-24 | 2017-05-31 | 天津双君智材科技发展有限公司 | Pitch crack autogenous healing microcapsules and preparation method thereof |
| CN108300423A (en) * | 2018-02-09 | 2018-07-20 | 苏州甫众塑胶有限公司 | A kind of preparation method of energy-efficient phase-change microcapsule |
| CN109738128A (en) * | 2018-12-29 | 2019-05-10 | 中国矿业大学 | For predicting Thermo-sensitive material, the preparation method and application of goaf coal spontaneous combustion |
| CN109758990A (en) * | 2019-03-19 | 2019-05-17 | 北京服装学院 | Preparation method and application with highly sensitive temperature induced color changing microcapsules |
| CN111100606A (en) * | 2019-12-30 | 2020-05-05 | 深圳先进电子材料国际创新研究院 | Low-temperature composite phase change energy storage material and preparation method and application thereof |
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| CN106350018A (en) * | 2016-07-29 | 2017-01-25 | 上海应用技术学院 | Water-free microwave heating energy-storing microcapsule with hot compress function and preparation method |
| CN106732222A (en) * | 2017-03-24 | 2017-05-31 | 天津双君智材科技发展有限公司 | Pitch crack autogenous healing microcapsules and preparation method thereof |
| CN108300423A (en) * | 2018-02-09 | 2018-07-20 | 苏州甫众塑胶有限公司 | A kind of preparation method of energy-efficient phase-change microcapsule |
| CN109738128A (en) * | 2018-12-29 | 2019-05-10 | 中国矿业大学 | For predicting Thermo-sensitive material, the preparation method and application of goaf coal spontaneous combustion |
| CN109738128B (en) * | 2018-12-29 | 2020-10-02 | 中国矿业大学 | Temperature-sensitive material for predicting spontaneous combustion of coal in goaf, preparation method and application |
| CN109758990A (en) * | 2019-03-19 | 2019-05-17 | 北京服装学院 | Preparation method and application with highly sensitive temperature induced color changing microcapsules |
| CN111909516A (en) * | 2019-05-09 | 2020-11-10 | 深圳光启岗达创新科技有限公司 | Heat-conducting composite material and preparation method thereof |
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| CN111100606B (en) * | 2019-12-30 | 2021-04-23 | 深圳先进电子材料国际创新研究院 | Low-temperature composite phase change energy storage material and preparation method and application thereof |
| CN111100606A (en) * | 2019-12-30 | 2020-05-05 | 深圳先进电子材料国际创新研究院 | Low-temperature composite phase change energy storage material and preparation method and application thereof |
| CN111518522A (en) * | 2020-06-09 | 2020-08-11 | 长沙理工大学 | Preparation method of graphite modified phase-change microcapsule |
| CN114214038A (en) * | 2021-12-30 | 2022-03-22 | 长安大学 | Paraffin/organic shell material phase change microcapsule for asphalt pavement and preparation method thereof |
| CN115094639A (en) * | 2022-06-13 | 2022-09-23 | 深圳市兴业卓辉实业有限公司 | Novel temperature-adjusting breathable fabric for protective clothing and preparation method thereof |
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