CN102876297B - A kind of low condensate depression phase-change material micro-capsule and preparation method thereof - Google Patents
A kind of low condensate depression phase-change material micro-capsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of low condensate depression phase-change material micro-capsule and preparation method thereof, its microcapsule are made up of capsule-core and cyst wall two portions, count by weight percentage, described capsule-core and cyst wall are respectively 30-85% and 15-70%, wherein: the moiety of capsule-core and weight percentage thereof are: organic phase change material 83-99.7%, excessively cold inhibitor 0.1-16%, initiator 0.1-0.5%; The moiety of cyst wall is: the multipolymer of alkyl methacrylate/aryl ester 80-95% and allyl ester class linking agent 5-20%.It is low that the phase-change material micro-capsule of microcapsule of the present invention has condensate depression, the features such as excellent property; This preparation method's technique is simple, easy to operate, applied widely, is convenient to industrial implementation.
Description
Technical field
The invention belongs to phase change material technical field, relate to a kind of phase-change material micro-capsule and preparation method thereof, be specifically related to a kind of low condensate depression phase-change material micro-capsule and preparation method thereof.
Background technology
Phase change material is the heat absorption and release phenomenon utilizing some exotic materials in phase transition process, thus carries out control and the temperature adjustment of heat.These materials with heat accumulation and adjusting control function are commonly referred to phase change material (Phase Change Material is called for short PCM).Phase transition process is a kind of isothermal or nearly quasi-isothermal process, and is attended by absorption or the release of larger heat in this process.The material that phase-changing energy storage material utilizes these special needs the character absorbing (or releasing) amount of heat to regulate and control energy when undergoing phase transition.According to the difference of material composition, phase change material can be divided into inorganic phase-changing material, organic phase change material and polymeric phase change material; Difference according to phase transformation mode can be divided into solid-liquid phase change material and solid-solid phase transition material.Different phase change material respectively has its different feature, and application also has some limitations.Microcapsulary is introduced phase change material by microencapsulated phase change material, increases heat transfer area, prevents the reaction of phase change material and surrounding environment, controls the volume change of PCM during phase in version, improves the service efficiency of phase change material, has broad application prospects.
Microcapsulary refers to and makes solid and liquid adopt filmogen to be rolled into the method for the particulate of nucleocapsid structure, and product pellet is called microcapsule.The size of general microcapsule is between 2 μm ~ 1000 μm scopes, and the thickness of shell is not at 0.2 μm ~ 10 μm etc.The surface shape of microcapsule is enriched, and mostly is spherical.The method of micro encapsulation originates from the 1950's, alters a great deal in decades afterwards.The solid-liquid phase change material that can be used as microcapsule inner core materials at present has crystalline hydrate salt, eutectic salt hydrate, straight-chain paraffin, paraffin class, fatty acid and polyoxyethylene glycol etc.The outside coating film for film forming material formation of microcapsule, is called wall material (also referred to as adventitia, cyst wall).Wall material is generally synthesized polymer material, and available wall material has polyethylene, polystyrene, polyureas, polymeric amide, epoxy resin, urea-formaldehyde resin, melamine formaldehyde resin etc.In addition, also containing other auxiliary agent such as nucleator in some microencapsulated phase change material, be used for improving the performance of phase change material.At present, phase change material is micro-/and Na capsule has been applied in sun power and nuclear energy, electronics, aircraft, the contour sophisticated technology domain variability of aerospace craft in fields such as heat-accumulation temperature-adjustment textiles, energy-saving building material, coating, and are expected to the biological fields such as the moist heat control being applied in plant seed.
The excessively cold method of current elimination phase-change material micro-capsule has two kinds: one to be add inspissated wax in phase change material, utilizes the crystallization of the inspissated wax nucleus induced phase transition materials first generated in crystallisation process; Two is the heterogeneous nucleation agent adding solid.But this two method has distinct disadvantage: (1) adds the amount of inspissated wax sufficiently large (generally needing 10-20 % by weight or more), like this certainly will to reduce the amount of effective constituent phase change material for cost; (2) problem brought that adds of heterogeneous nucleation agent to reduce the packing rate of microcapsule on the one hand, on the other hand, also must solve the problems such as the dispersion stabilization of heterogeneous nucleation agent particle in phase change material.
Therefore, preparing a kind of amount neither affecting effective constituent phase change material avoids again the phase-change material micro-capsule of the efficient low condensate depression of the loaded down with trivial details dispersion process of heterogeneous nucleation agent in phase change material to remain the difficult point of current phase-change material micro-capsule research field, and the breakthrough in this direction has important strategic importance to the application promoting phase-change material micro-capsule.
Summary of the invention
The object of the invention is to overcome above-mentioned technological deficiency, provide a kind of low condensate depression phase-change material micro-capsule and preparation method thereof, it is low that the phase-change material micro-capsule of these microcapsule has condensate depression, the features such as excellent property; This preparation method's technique is simple, easy to operate, applied widely, is convenient to industrial implementation.Its technical scheme is:
A kind of low condensate depression phase-change material micro-capsule, its microcapsule are made up of capsule-core and cyst wall two portions, count by weight percentage, and described capsule-core and cyst wall are respectively 30-85% and 15-70%, wherein:
The moiety of capsule-core and weight percentage thereof are: organic phase change material 83-99.7%, excessively cold inhibitor 0.1-16%, initiator 0.1-0.5%;
The moiety of cyst wall is: the multipolymer of alkyl methacrylate/aryl ester 80-95% and allyl ester class linking agent 5-20%.
Described organic phase change material refers to general formula C
nh
2n+2(n=12-32) the normal paraffin compounds represented, with general formula C
nh
2n+2the halo normal paraffin compounds that X (n=12-32) represents and with general formula C
mh
2m+1cOOCH
2c
ph
2p+1any 1 ~ 3 kind in the fatty acid ester that (n=12-32, m=10-20, p=4-10) represents;
The cold inhibitor of described mistake refers to polypyrrole;
Described initiator refers to Diisopropyl azodicarboxylate;
Described oxygenant refers to benzoyl peroxide;
Described alkyl methacrylate/aryl ester refers to general formula:
1-3 kind in the acrylate of (in formula, R is methyl, ethyl, propyl group, butyl, hexyl, decyl, lauryl, cyclohexyl, methylcyclohexyl, phenyl, benzyl);
Described allyl ester class linking agent refers to allyl methacrylate(AMA), Ethylene glycol dimethacrylate, diethyleneglycol dimethacrylate(DEGDMA), TEGDMA, dimethacrylate TEG ester, dimethacrylate 1,3-butanediol ester, dimethacrylate 1, at least one in 4-butanediol ester, dimethacrylate 1,6-hexylene glycol ester, trihydroxy methyl propane trimethyl acrylate, neopentyl glycol dimethacrylate, Ethoxylated bisphenol A dimethacrylate.
A preparation method for low condensate depression phase-change material micro-capsule, comprises following steps:
(1) preparation of oil mixture:
By organic phase change material, cross cold inhibitor monomer, initiator, oxygenant, alkyl methacrylate/aryl ester, allyl ester class linking agent mixs, are heated to above organic phase change material melt temperature 10-20 DEG C of scope in ratio according to claim 2, stirring makes it to dissolve completely and presents water white mixed solution;
(2) preparation of aqueous mixture:
Be dispersed in water as aqueous phase using emulsifying agent and assistant for emulsifying agent, wherein emulsifying agent solid content is 0.5-4%, and assistant for emulsifying agent accounts for 0.1-2% with the total weight of aqueous phase;
(3) preparation of emulsion:
Shear with refiner, oil phase is dispersed in aqueous phase and forms O/W emulsion, velocity of shear is 3000-8000 rev/min;
(4) preparation of microcapsule:
Transfer in reactor by the O/W emulsion that step (3) obtains, adopt paddle to stir, stirring velocity is 30-500 rev/min, after reacting 3-4 hour, namely obtains phase-change material micro-capsule under heating in water bath to 60-68 DEG C of temperature;
(5) preparation of the cold phase-change material micro-capsule of low mistake:
Step (4) is obtained phase-change material micro-capsule to continue to be warmed up to 75-85 DEG C of reaction after 1-2 hour, naturally cooling, namely obtains the cold phase-change material micro-capsule of low mistake.
Emulsifying agent described in step (2) is styrene-maleic anhydride copolymer, and described assistant for emulsifying agent is n-Octanol.
Oil mixture described in step (1) accounts for the 10-30% of the described emulsion gross weight of step (3).
Compared with prior art, beneficial effect of the present invention is:
Technical scheme of the present invention added cold inhibitor monomer in the preparation of microcapsule, due to the existence of oxygenant in preparation process, in-situ preparation is dispersed in the small mistake cold inhibitor particle in phase change material, the crystallization of phase change material is carried out towards the direction of heterogeneous nucleation, inhibits serious cold crystallization excessively.Be in-situ preparation after microcapsule are formed owing to crossing cold inhibitor, avoid the problems such as the encapsulated productive rate that the cold inhibitor of additional mistake brings is low, particle adhesion.Operating process is simple, does not lump, and the microcapsule obtained after using allyl ester class linking agent have more pliable and tougher shell, and surface has and subsides and gauffer, can alleviate volume change when phase change material undergoes phase transition to the pressure of shell material.Except adding the cold inhibitor monomer of a small amount of mistake, do not mix other materials in microcapsule preparation, therefore obviously can not reduce the heat storage capacity of microcapsule.
Accompanying drawing explanation
Fig. 1. be the electron scanning micrograph figure of the cold phase-change material micro-capsule embodiment 1 of the low mistake of the present invention;
Fig. 2. for the DSC of the cold phase-change material micro-capsule embodiment 3-6 of the low mistake of the present invention schemes, wherein: a-pyrroles 0%; B-pyrroles 4%; C-pyrroles 8%; D-pyrroles 12%; The pure phase change material of e-(experiment condition: N
2atmosphere, sweep velocity 10 DEG C/minute).
Embodiment
Below in conjunction with accompanying drawing and embodiment, technical scheme of the present invention is described in more detail.
Embodiment 1
Microcapsule mass percent composition is designed to:
Capsule-core 128g, wherein organic phase change material Octadecane 120g, cross cold inhibitor polypyrrole 5g, initiator Diisopropyl azodicarboxylate (AIBN) 1.5g, oxygenant benzoyl peroxide (BPO) 1.5g; Cyst wall 110g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 100g and 10g.
The preparation method of microcapsule is:
(1) preparation of oil mixture: at the temperature of 45 DEG C and under the stirring velocity of 300 revs/min, the organic phase change material of described quality, excessively cold inhibitor monomer, initiator, oxygenant, alkyl methacrylate/aryl ester, allyl ester class linking agent are mixed in proportion and stir, makes oil mixture;
(2) preparation of aqueous mixture: take 2000g water, 100gTA (the styrene-maleic anhydride copolymer sodium-salt aqueous solution of 19%, be purchased from Shanghai Leather Chemical Plant) and 10g n-Octanol in 5L glass reaction still, the also heating in water bath that stirs, to 45 DEG C, makes aqueous mixture; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 10.1%;
(3) preparation of emulsion: refiner cutting head is placed in aqueous mixture, regulates velocity of shear to be 3000 revs/min, and emulsification times is formed evenly for 10 minutes;
(4) preparation of microcapsule: the temperature of O/W emulsion emulsion is risen to 68 DEG C, opens blade stirring and regulates stirring velocity to be 300 revs/min, react and complete for 3 hours, make phase-change material micro-capsule;
(5) preparation of the cold phase-change material micro-capsule of low mistake: phase-change material micro-capsule will be obtained and continue to be warmed up to 78 DEG C of maintenances 1 hour, and observe microcapsule suspensions and become grey black gradually, naturally cooling, namely obtain the cold phase-change material micro-capsule of low mistake.Stop stirring, cooling water circulation is to room temperature, and filtering separation, after the deionized water rinsing product 3 times of quality 1000g, is dried to constant weight, namely obtains phase-change material micro-capsule dry powder in 50 DEG C of vacuum drying ovens.
After testing, the median size of gained phase-change material micro-capsule is 15.2 μm, endothermic temperature (Tm) 28.1 DEG C, melting enthalpy (Δ Hm) 118.3J/g, exothermic temperature (Tc3) 22.8 DEG C, crystallization heat content (Δ Hc3) 28.3J/g, exothermic temperature (Tc2) 17.6 DEG C, crystallization heat content (Δ Hc2) 4.8J/g, exothermic temperature (Tc1) 11.7 DEG C, crystallization heat content (Δ Hc1) 3.3J/g; Heat decomposition temperature (Td) 227 DEG C (data of thermal weight loss 5%).
Embodiment 2
Microcapsule mass percent composition is designed to:
Capsule-core 263g, wherein organic phase change material 1-bromo eicosane 240g, cross cold inhibitor polypyrrole 15g, initiator Diisopropyl azodicarboxylate (AIBN) 1g, oxygenant benzoyl peroxide (BPO) 1g; Cyst wall 320g, wherein phenyl methacrylate and linking agent dimethacrylate TEG ester are respectively 300g and 20g.
The preparation method of microcapsule is:
(1) preparation of oil mixture: at the temperature of 55 DEG C and under the stirring velocity of 500 revs/min, the organic phase change material of described quality, excessively cold inhibitor monomer, initiator, oxygenant, alkyl methacrylate/aryl ester, allyl ester class linking agent are mixed in proportion and stir, makes oil mixture;
(2) preparation of aqueous mixture: take 1800g water, 150gTA (the styrene-maleic anhydride copolymer sodium-salt aqueous solution of 19%, be purchased from Shanghai Leather Chemical Plant) and 10g n-Octanol in 5L glass reaction still, the also heating in water bath that stirs, to 55 DEG C, makes aqueous mixture;
(3) preparation of emulsion: refiner cutting head is placed in aqueous mixture, regulates velocity of shear to be 8000 revs/min, and emulsification times is formed evenly for 10 minutes; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 23%;
(4) preparation of microcapsule: the temperature of O/W emulsion emulsion is risen to 65 DEG C, opens blade stirring and regulates stirring velocity to be 400 revs/min, react and complete for 4 hours, make phase-change material micro-capsule;
(5) preparation of the cold phase-change material micro-capsule of low mistake: phase-change material micro-capsule will be obtained and continue to be warmed up to 75 DEG C of maintenances 2 hours, and observe microcapsule suspensions and become grey black gradually, naturally cooling, namely obtain the cold phase-change material micro-capsule of low mistake.Stop stirring, cooling water circulation is to room temperature, and filtering separation, after the deionized water rinsing product 3 times of quality 1000g, is dried to constant weight, namely obtains phase-change material micro-capsule dry powder in 50 DEG C of vacuum drying ovens.
After testing, the median size of gained phase-change material micro-capsule is 3.2 μm, endothermic temperature (Tm) 34.1 DEG C, melting enthalpy (Δ Hm) 115J/g, exothermic temperature (Tc3) 25.2 DEG C, crystallization heat content (Δ Hc3) 21.8J/g, exothermic temperature (Tc2) 19.6 DEG C, crystallization heat content (Δ Hc2) 3.6J/g, exothermic temperature (Tc1) 13.5 DEG C, crystallization heat content (Δ Hc1) 2.8J/g; Heat decomposition temperature (Td) 237 DEG C (data of thermal weight loss 5%).
Embodiment 3 ~ 7
Adopt the processing condition identical with embodiment 1, only change the content of pyrroles, obtain the cold phase-change material micro-capsule of low mistake that polypyrrole content is different, its performance is as shown in table 1.The composition of embodiment 3 ~ 7 microcapsule is respectively:
Embodiment 3
Capsule-core 295.2g, wherein organic phase change material 280g, cross cold inhibitor 0g, initiator 1.2g, oxygenant 1.0g; Cyst wall 115g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 100g and 15g; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 16%;
Embodiment 4
Capsule-core 377.2g, wherein organic phase change material 360g, cross cold inhibitor 15g, initiator 1.2g, oxygenant 1.0g; Cyst wall 115g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 100g and 15g; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 19%;
Embodiment 5
Capsule-core 395.2g, wherein organic phase change material 360g, cross cold inhibitor 32g, initiator 1.2g, oxygenant 1.0g; Cyst wall 240g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 220g and 20g; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 23.2%;
Embodiment 6
Capsule-core 412.2g, wherein organic phase change material 360g, cross cold inhibitor 50g, initiator 1.2g, oxygenant 1.0g; Cyst wall 320g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 290g and 30g; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 25.8%;
Embodiment 7
Capsule-core 432.2g, wherein organic phase change material 400g, cross cold inhibitor 77g, initiator 1.2g, oxygenant 1.0g; Cyst wall 330g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 300g and 30g; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 27.7%;
Table 1 difference crosses the performance table of cold inhibitor polypyrrole phase-change material micro-capsule
Data as can be seen from table 1, along with the increase of crossing cold inhibitor, Δ Hc1, Δ Hc2 are in reduction, and Δ Hc3 increases, but when crossing cold inhibitor more than 10%, Δ Hc1, Δ Hc2 increase again gradually, and Δ Hc3 reduces; Along with oil mixture accounts for the increase of emulsion gross weight mark, there will be reunion and caking phenomenon.
Embodiment 8
Capsule-core 263g, wherein organic phase change material n-butyl stearate 300g, cross cold inhibitor polypyrrole 15g, initiator Diisopropyl azodicarboxylate (AIBN) 1g, oxygenant benzoyl peroxide (BPO) 1g; Cyst wall 200g, wherein butyl methacrylate and linking agent dimethacrylate BDO ester are respectively 300g and 20g.
The preparation method of microcapsule is:
(1) preparation of oil mixture: at the temperature of 40 DEG C and under the stirring velocity of 500 revs/min, the organic phase change material of described quality, excessively cold inhibitor monomer, initiator, oxygenant, alkyl methacrylate/aryl ester, allyl ester class linking agent are mixed in proportion and stir, makes oil mixture;
(2) preparation of aqueous mixture: take 1800g water, 150gTA (the styrene-maleic anhydride copolymer sodium-salt aqueous solution of 19%, Shanghai Leather Chemical Plant) and 5g n-Octanol in 5L glass reaction still, the also heating in water bath that stirs, to 40 DEG C, makes aqueous mixture;
(3) preparation of emulsion: refiner cutting head is placed in aqueous mixture, regulates velocity of shear to be 5000 revs/min, and emulsification times is formed evenly for 20 minutes; In the present embodiment, oil mixture accounts for emulsion gross weight mark is 23%;
(4) preparation of microcapsule: the temperature of O/W emulsion emulsion is risen to 66 DEG C, opens blade stirring and regulates stirring velocity to be 300 revs/min, react and complete for 3.5 hours, make phase-change material micro-capsule;
(5) preparation of the cold phase-change material micro-capsule of low mistake: phase-change material micro-capsule will be obtained and continue to be warmed up to 85 DEG C of maintenances 1 hour, and observe microcapsule suspensions and become grey black gradually, naturally cooling, namely obtain the cold phase-change material micro-capsule of low mistake.Stop stirring, cooling water circulation is to room temperature, and filtering separation, after the deionized water rinsing product 3 times of quality 1000g, is dried to constant weight in 50 DEG C of vacuum drying ovens.
After testing, the median size of gained phase-change material micro-capsule is 5.8 μm, endothermic temperature (Tm) 23.1 DEG C, melting enthalpy (Δ Hm) 69J/g, exothermic temperature (Tc3) 13.1 DEG C, crystallization heat content (Δ Hc3) 34.8J/g, exothermic temperature (Tc2) 8.9 DEG C, crystallization heat content (Δ Hc2) 4.6J/g, exothermic temperature (Tc1) 3.5 DEG C, crystallization heat content (Δ Hc1) 29.8J/g; Heat decomposition temperature (Td) 227 DEG C (data of thermal weight loss 5%).
The above; be only the present invention's preferably embodiment; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the simple change of the technical scheme that can obtain apparently or equivalence are replaced and are all fallen within the scope of protection of the present invention.
Claims (1)
1. a low condensate depression phase-change material micro-capsule, is characterized in that, the raw material packet preparing described microcapsule contains:
Capsule-core 128g, wherein organic phase change material Octadecane 120g, cross cold inhibitor pyrrole 5g, initiator Diisopropyl azodicarboxylate AIBN1.5g, oxygenant benzoyl peroxide BPO1.5g; Cyst wall 110g, wherein methyl methacrylate and linking agent allyl methacrylate(AMA) are respectively 100g and 10g;
The preparation method of described low condensate depression phase-change material micro-capsule is:
(1) preparation of oil mixture: at the temperature of 45 DEG C and under the stirring velocity of 300 revs/min, the organic phase change material of described quality, excessively cold inhibitor monomer, initiator, oxygenant, methyl methacrylate, linking agent allyl methacrylate(AMA) are mixed in proportion and stir, makes oil mixture;
(2) preparation of aqueous mixture: take 2000g water, 100gTA and 10g n-Octanol in 5L glass reaction still, stir and heating in water bath to 45 DEG C, make aqueous mixture, wherein TA is the styrene-maleic anhydride copolymer sodium-salt aqueous solution of 19%, is purchased from Shanghai Leather Chemical Plant;
(3) preparation of emulsion: shear with refiner, oil phase is dispersed in aqueous phase and forms O/W emulsion, velocity of shear is 3000 revs/min, and emulsification times forms uniform emulsion in 10 minutes, and it is 10.1% that oil mixture accounts for emulsion gross weight mark:
(4) preparation of microcapsule: the temperature of O/W emulsion is risen to 68 DEG C, opens blade stirring, regulates stirring velocity to be 300 revs/min, reacts and complete for 3 hours, make phase-change material micro-capsule;
(5) preparation of the cold phase-change material micro-capsule of low mistake: the phase-change material micro-capsule obtained is continued be warmed up to 78 DEG C and keep 1 hour, observe microcapsule suspensions and become grey black gradually, naturally cooling, namely obtain the cold phase-change material micro-capsule of low mistake; Stop stirring, cooling water circulation is to room temperature, and filtering separation, after the deionized water rinsing product 3 times of quality 1000g, is dried to constant weight, namely obtains phase-change material micro-capsule dry powder in 50 DEG C of vacuum drying ovens.
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| CN103805142B (en) * | 2013-12-30 | 2016-11-16 | 清华大学深圳研究生院 | A kind of silicon nitride modification microcapsules of storing energy through phase change and preparation method thereof |
| CN104962242B (en) * | 2015-06-26 | 2017-12-01 | 天津工业大学 | A kind of low degree of supercooling phase-change material micro-capsule and preparation method thereof |
| CN107815297B (en) * | 2017-11-13 | 2020-06-23 | 天津工业大学 | Green environment-friendly microcapsule and preparation method thereof |
| CN110746938B (en) * | 2019-10-17 | 2021-05-11 | 东华大学 | Cellulose/polypyrrole supported composite phase change heat storage material and preparation method thereof |
| CN111072958A (en) * | 2019-12-03 | 2020-04-28 | 天津圣工科技有限公司 | Polypyrrole/melamine resin double-shell structure microcapsule and preparation method thereof |
| CN110951465A (en) * | 2019-12-13 | 2020-04-03 | 天津优米优科技有限公司 | Novel phase change capsule and preparation method thereof |
| CN113355056A (en) * | 2021-06-22 | 2021-09-07 | 广西民族大学 | Preparation method of photo-thermal phase change energy storage micro-nano super-hydrophobic anti-freezing particle material |
| CN113913160B (en) * | 2021-11-09 | 2023-08-15 | 青岛尼希米生物科技有限公司 | Double-layer capsule wall energy storage temperature adjustment microcapsule, polyacrylonitrile fiber and preparation method thereof |
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