CN104962240A - Preparation method of nano particle-doped phase change microcapsule - Google Patents
Preparation method of nano particle-doped phase change microcapsule Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano particle-doped phase change microcapsule. The preparation method comprises following steps: a nano material is subjected to surface treatment, and then is added into a core material after surface treatment so as to obtain a composite nano core material emulsion; a prepared prepolymer capsule wall material is added into the nano core material emulsion so as to obtain a capsule suspension liquid loaded with the nano material; and the capsule suspension liquid is subjected to filtering, washing, drying, and grinding so as to obtain nano particle-doped phase change microcapsule powder. According to the preparation method, the functional nano material is subjected to pretreatment, and then is doped into a shell material or the core material of the microcapsule, so that synergistic effects with a phase change material in the microcapsule are achieved; and loading amount of the nano particle on different parts of the microcapsule is controlled by controlling surface energy of the nano material, and further more nano composite phase change material microcapsules with a plurality of functions (heat functions, optical functions, magnetic functions, and electric function) are prepared.
Description
Technical field
The invention belongs to phase change material technical field, be specifically related to a kind of preparation method of phase-change microcapsule of doped with nanometer particle.
Background technology
Energy shortage and environmental problem enjoy the concern of various circles of society always, energy-conserving and environment-protective, improve efficiency of energy utilization, have become the emphasis of various countries working energy person research and development.Latent heat heat-storage technology is attractive especially in energy utilization, phase change material (PCM) is as a kind of high-level efficiency hidden heat energy storage medium, can in its thing phase change process, absorb heat (cold) amount from environment or release heat (cold) amount to environment, thus reaching the object of energy storage and release.
In phase-changing energy storage material research field, having occurred a new trend in recent years, is namely one of wall material component synthesis phase-changing energy storage material capsule with inorganic materials.Inorganic materials has the features such as the incomparable high strength of polymkeric substance, flame retardancy, high thermal stability, high thermal conductivity and dense materials are high, and capsule wall is also better to the protected effect of phase change material.Therefore effectively can improve the defects such as conventional phase change material microcapsule easily break, easily leakage, easily loss, greatly improve permeability resistance and flame retardant resistance, thus significantly improve its work-ing life and reliability.
Along with going deep into of research, we find that organic/inorganic microcapsule phase-change energy storage material is except the heat storage function with core, the specific physical chemical efficiency of its wall material is also worth deeply exploitation, adulterate a certain amount of nanoparticle in phase change material, defines a kind of advanced composite material--nano-composite phase-changing material.Because nanoparticle has large specific surface area and strong interfacial effect, thus make the composite material exhibits of doped with nanometer particle go out to be different from the mechanics of general macrocomposite, calorifics, electricity, magnetics and optical property, its performance not each component property simply adding and, but on the basis keeping each constituent materials fundamental property, have the over-all properties that stock blend does not possess, be a kind of brand-new new and high technology material, there is excellent performance and wide prospect.
Summary of the invention
The object of this invention is to provide a kind of preparation method of phase-change microcapsule of doped with nanometer particle, by dopen Nano powder in microcapsule core material, prepare the microencapsulated phase change material of mechanics, calorifics, electricity, magnetics or excellent optical performance, solve the problem of existing nano capsule phase change material function singleness.
The technical solution adopted in the present invention is, a kind of preparation method of phase-change microcapsule of doped with nanometer particle, and concrete steps are as follows:
Step 1, nano-material surface process:
Surface treatment agent alcoholic solvent is diluted to the solution that concentration is 5 ~ 20%, regulates its pH value to 4 ~ 5 with the acetum of 10%, stirring at normal temperature process 10min, obtains surface treatment agent solution; Surface treatment agent solution is joined in nano material, after stirring reaction 20min, be warming up to 50 ~ 60 DEG C, insulation reaction 20min ~ 30min, after product suction filtration, is placed in the drying in oven of 60 DEG C ~ 65 DEG C, nanometer powder after must processing after cooling grinding, for subsequent use;
Step 2, the preparation of cyst material:
By trimeric cyanamide and formaldehyde mixing, at 70 DEG C of stirring reaction 30 ~ 50min, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 3, nano material is adulterated:
Core material is placed heated and stirred in the water-bath with 50 DEG C and make its melting, get sodium salt that pH is the polystyrene-maleic acyl multipolymer of 7 or ammonium salt joins in core material, add step 1 gained nanometer powder, start high-shear emulsion machine with 3500 ~ 4000rpm, emulsification 20min ~ 30min, obtains the core material emulsion of composite nano materials;
Prepared by step 4. Nano capsule suspension:
Step 2 gained performed polymer is joined in step 3 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 200 ~ 300rpm, add the PH to 5 that acetic acid regulates emulsion, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 3 ~ 4h under Keep agitation, adjusting PH with 10% sodium carbonate solution is 7, after termination reaction, obtains the capsule suspension liquid of loaded with nano material;
Step 5. doped nano-material phase-change microcapsule powder is refined:
Step 4 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of loaded with nano material.
Feature of the present invention is also,
In step 1, alcoholic solvent is one in ethanol, methyl alcohol or Virahol or mixture.
In step 1, surface treatment agent is the one in 3-methacryloxypropyl trimethoxy silane, methyltrimethoxy silane, Union carbide A-162 octyltri-ethoxysilane, 3-mercaptopropyltriethoxysilane, trimethyl siloxanes, methyl trimethoxy oxygen radical siloxane, aminopropyl trimethoxysilane or vinyltrimethoxy silane.
In step 1, nano material is one in nano titanium oxide, nano stibium doped tin oxide, nano zine oxide, carbon nanotube, nano silicon, nanometer silicon carbide, nanometer iron powder, copper nanoparticle, nanometer aluminium powder, nano-nickel powder, nano-silver powder, nano-cerium oxide powder or nano lanthanum oxide powder or mixture.
In step 1, the consumption of surface treatment agent solution is 1 ~ 10 times of nano material consumption.
In step 2, the mass concentration of formaldehyde is 37%, and the mol ratio of trimeric cyanamide and formaldehyde is 1:1.6 ~ 2.5.
In step 3, core material is the one in bromotetradecane, bromohexadecane, bromo-octadecane, bromo eicosane, n-tetradecane, n-hexadecane, Octadecane or NSC 62789.
In step 3, the sodium salt of polystyrene-maleic acyl or the molecular weight of ammonium salt are 60,000 ~ 130,000, and the mass ratio of the sodium salt of polystyrene-maleic acyl or ammonium salt and core material is 1:5 ~ 10.
In step 3, the consumption of nanometer powder is 0.5 ~ 20% of core material.
In step 4, the mass ratio of performed polymer and core material emulsion is 1:4 ~ 8.
The invention has the beneficial effects as follows, in the shell material being entrained in microcapsule after pre-treatment is carried out to functional nanomaterials or core material, make it to work in coordination with generating effect with the phase change material in microcapsule, and control nanoparticle in microcapsule each position charge capacity by the surface energy controlling nano material, and then prepare several functions (heat, light, magnetic, electricity) in the nano-composite phase-changing material microcapsule of one.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of the embodiment of the present invention 1 gained microcapsule;
Fig. 2 is the Electronic Speculum figure of the embodiment of the present invention 2 gained microcapsule;
Fig. 3 is the Electronic Speculum figure of comparative example gained microcapsule of the present invention;
Fig. 4 is the DSC figure of the embodiment of the present invention 2 gained microcapsule;
Fig. 5 is the DSC figure of comparative example gained microcapsule of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Step 1, nano-material surface process:
By 5.2g trimethyl siloxanes with after the dilution of 100mL alcohol solvent, regulate its pH value to 4 with the acetum of 10%, stirring at normal temperature process 10min, obtains surface treatment agent solution; Getting 6mL surface treatment agent solution joins in 6g P25 nano titanium oxide, after stirring reaction 20min, is warming up to 50 DEG C, insulation reaction 20min, after product suction filtration, is placed in the drying in oven of 60 DEG C, P25 nano titanium dioxide powder after must processing after cooling grinding, for subsequent use;
Step 2, the preparation of cyst material:
Be the formaldehyde mixing of 37% by 5.62g trimeric cyanamide and 5.06mL mass concentration, at 70 DEG C of stirring reaction 30min, become clear liquor, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 3, nano material is adulterated:
30g n-hexadecane is positioned over heated and stirred in the water-bath of 50 DEG C and makes its melting, getting 3g molecular weight is that the sodium salt deionized water of 130,000 polystyrene-maleic acyl multipolymers is diluted to 50g, pH is adjusted to be after 7 with 10% acetic acid, join in n-hexadecane, after stirring, add 0.15g step 1 gained nanometer powder, start high-shear emulsion machine with 3500rpm, emulsification 30min, obtains the core material emulsion of compound P25 nano titanium oxide;
Prepared by step 4. Nano capsule suspension:
Getting 10g step 2 gained performed polymer joins in 40g step 3 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 200rpm, add the PH to 5 of the acetic acid adjustment emulsion of 10%, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 3h under Keep agitation, adjusting PH with the sodium carbonate solution that concentration is 10% is 7, after termination reaction, obtains the phase-change microcapsule suspension of load P 25 nanometer titanic oxide material;
Step 5. mixed nanometer phase-change microcapsule powder is refined:
Step 4 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of load P 25 nanometer titanic oxide material.
The particle diameter of the microscapsule powder of the present embodiment gained load P 25 nanometer titanic oxide material is 5 ~ 8 μm, its Electronic Speculum figure as shown in Figure 1, as can be seen from the figure combine closely between P25 nano titanium oxide and microcapsule shell material, be combined on shell material, particle major part is dispersed in surface of microcapsule, have between nanoparticle and form netted connection trend mutually, the particle between microcapsule does not observe particle.
Embodiment 2
Step 1, nano-material surface process:
By 12g trimethyl siloxanes with after the dilution of 100mL alcohol solvent, regulate its pH value to 4.5 with the acetum of 10%, stirring at normal temperature process 10min, obtains surface treatment agent solution; Getting 30mL surface treatment agent solution joins in 6g P25 nano titanium oxide, after stirring reaction 20min, is warming up to 55 DEG C, insulation reaction 20min, after product suction filtration, is placed in the drying in oven of 63 DEG C, P25 nano titanium dioxide powder after must processing after cooling grinding, for subsequent use;
Step 2, the preparation of cyst material:
Be the formaldehyde mixing of 37% by 8.12g trimeric cyanamide and 10.46mL mass concentration, at 70 DEG C of stirring reaction 30min, become clear liquor, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 3, nano material is adulterated:
30g n-hexadecane is positioned over heated and stirred in the water-bath of 50 DEG C and makes its melting, getting 5g molecular weight is that the sodium salt deionized water of 90,000 polystyrene-maleic acyl multipolymers is diluted to 50g, pH is adjusted to be after 7 with 10% acetic acid, join in n-hexadecane, after stirring, add 3g step 1 gained nanometer powder, start high-shear emulsion machine with 3800rpm, emulsification 25min, obtains the core material emulsion of compound P25 nano titanium oxide;
Prepared by step 4. Nano capsule suspension:
Getting 10g step 2 gained performed polymer joins in 60g step 3 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 280rpm, add the PH to 5 of the acetic acid adjustment emulsion of 10%, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 3.5h under Keep agitation, adjusting PH with the sodium carbonate solution that concentration is 10% is 7, after termination reaction, obtains the phase-change microcapsule suspension of load P 25 nanometer titanic oxide material;
Step 5. mixed nanometer phase-change microcapsule powder is refined:
Step 4 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of load P 25 nanometer titanic oxide material.
The particle diameter of the microcapsule of the present embodiment gained load P 25 nanometer titanic oxide material is 5 ~ 8 μm, its Electronic Speculum figure as shown in Figure 2, as can be seen from the figure, combine closely between P25 nano-titania particle and microcapsule shell material, visible much bury fall into enter shell material inside, particle major part is dispersed in surface of microcapsule, and the particle between microcapsule does not observe particle; Under this state, the thermostability of phase-change microcapsule is best, and surfusion is inhibited, and DSC figure as shown in Figure 4.
Embodiment 3
Step 1, nano-material surface process:
By 25g octyl group Trimethoxy silane with after the dilution of 100mL methanol solvate, regulate its pH value to 5 with the acetum of 10%, stirring at normal temperature process 10min, obtains surface treatment agent solution; Getting 60mL surface treatment agent solution joins in 6g P25 nano titanium oxide, after stirring reaction 20min, is warming up to 60 DEG C, insulation reaction 20min, after product suction filtration, is placed in the drying in oven of 65 DEG C, P25 nano titanium dioxide powder after must processing after cooling grinding, for subsequent use;
Step 2, the preparation of cyst material:
Be the formaldehyde mixing of 37% by 2.35g trimeric cyanamide and 7.6mL mass concentration, at 70 DEG C of stirring reaction 50min, become clear liquor, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 3, nano material is adulterated:
30g Octadecane is positioned over heated and stirred in the water-bath of 50 DEG C and makes its melting, getting 6g molecular weight is that the sodium salt deionized water of 60,000 polystyrene-maleic acyl multipolymers is diluted to 50g, pH is adjusted to be after 7 with 10% acetic acid, join in Octadecane, after stirring, add 6g step 1 gained nanometer powder, start high-shear emulsion machine with 4000rpm, emulsification 20min, obtains the core material emulsion of compound P25 nano titanium oxide;
Prepared by step 4. Nano capsule suspension:
Getting 10g step 2 gained performed polymer joins in 80g step 3 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 300rpm, add the PH to 5 of the acetic acid adjustment emulsion of 10%, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 4h under Keep agitation, adjusting PH with the sodium carbonate solution that concentration is 10% is 7, after termination reaction, obtains the phase-change microcapsule suspension of load P 25 nanometer titanic oxide material;
Step 5. mixed nanometer phase-change microcapsule powder is refined:
Step 4 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of load P 25 nanometer titanic oxide material.
The particle diameter of the microcapsule of the present embodiment gained load P 25 nanometer titanic oxide material is 5 ~ 8 μm.
Comparative example
Step 1, the preparation of cyst material:
Be the formaldehyde mixing of 37% by 8.12g trimeric cyanamide and 10.46mL mass concentration, at 70 DEG C of stirring reaction 30min, become clear liquor, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 2, nano material is adulterated:
Be that the sodium salt deionized water of 80,000 polystyrene-maleic acyl multipolymers is diluted to 50g by 5g molecular weight, pH is adjusted to be after 7 with 10% acetic acid, join in 30g bromotetradecane, stir and add 3g Beijing and receive the undressed nanometer anatase titania powder of occasion, start high-shear emulsion machine with 3800rpm, emulsification 25min, obtains the core material emulsion of composite nano titanium dioxide;
Prepared by step 3. Nano capsule suspension:
Getting 10g step 1 gained performed polymer joins in 60g step 2 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 280rpm, add the PH to 5 of the acetic acid adjustment emulsion of 10%, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 3.5h under Keep agitation, adjusting PH with the sodium carbonate solution that concentration is 10% is 7, after termination reaction, obtains the phase-change microcapsule suspension of load nano-titanium dioxide material;
Step 4. mixed nanometer phase-change microcapsule powder is refined:
Step 3 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of load nano-titanium dioxide material.
The particle diameter of the microcapsule of the present embodiment gained load nano-titanium dioxide material is 10 ~ 12 μm, its Electronic Speculum figure as shown in Figure 3, as can be seen from the figure be combined without essence between nano-titania particle with microcapsule shell material, particle major part is dispersed between microcapsule and is deposited on surface of microcapsule, disperse between microcapsule, there is no adhesion phenomenon; Its DSC schemes as shown in Figure 5.
The present invention utilizes the core/shell structure of phase-change material micro-capsule uniqueness, doping commodity nano material, prepare composite phase-change microcapsule, promote the performance of phase-change microcapsule, the phase-change material micro-capsule wall material that the principle of invention is to be in semi-crystalline can adulterate various metallic element and inorganic oxide, non-metallic element, various rare earth oxide, Graphene, CNT (carbon nano-tube), graphite, ATO powder, nano-silver powder etc., prepared phase-change microcapsule is except having thermal conditioning performance, in heat conduction, suppress superfusibility, thermostability aspect is all improved to some extent, in addition due to the performance of dopant material, functional design can be carried out to phase-change microcapsule, give microencapsulation material additional function according to materials application occasion, namely except phase-change accumulation energy and these traditional functions of temperature buffer, such as uvioresistant can also be given, the optical properties such as visible ray-infrared ray absorption reflection, and the function that antibacterial bacteriostatic performance etc. is additional, by functional powder (commodity) load in polymer shell material microcapsule, functional nanomaterials is then disperseed and is fixed, nano-functional material and micrograde polymer microsphere are combined into be integrated, so just can solve the agglomeration traits of nano material, and it can be facilitated to recycle, its using value can increase considerably, and can be widely used in the multiple fields such as sun power, aerospace, building, weaving, electric power, sewage disposal.
The present invention carries out surface treatment to nanoparticle, makes a certain composition in itself and microcapsule affine or repel, and so as to the distribution of manipulation nanoparticle at each position of microcapsule, optimizes the various application performances of phase-change microcapsule to greatest extent; By the performance of nano material excellence, functional design is carried out to phase-change microcapsule, make it more intelligent, by the various heterogeneity nanoparticle that adulterates, make there is synergistic effect between microcapsule functions; Simultaneously because nano material specific surface area is large, surface energy is very high, and organic polymer wall material and core surfaces can be low usually, want the combination that the two has had, surface treatment must be carried out to the material that will adulterate, when adopting surface treatment, be worked out by technique, surface treatment degree needs controllable precise, object be make the shell material of itself and phase-change microcapsule or a certain composition compatible; Experimental data proves the height of degree for the treatment of, that is surface energy size finally can have impact to the distribution of nano material in microcapsule structure and charge capacity, and then nano material doping has great impact to the final performance of material, to relation (thermostability between nano load amount and its various application performance, cross cold, heat enthalpy value, photocatalysis performance etc.) systematic study highly significant.
Claims (10)
1. a preparation method for the phase-change microcapsule of doped with nanometer particle, is characterized in that, concrete steps are as follows:
Step 1, nano-material surface process:
Surface treatment agent alcoholic solvent is diluted to the solution that concentration is 5 ~ 20%, regulates its pH value to 4 ~ 5 with the acetum of 10%, stirring at normal temperature process 10min, obtains surface treatment agent solution; Surface treatment agent solution is joined in nano material, after stirring reaction 20min, be warming up to 50 ~ 60 DEG C, insulation reaction 20min ~ 30min, after product suction filtration, is placed in the drying in oven of 60 DEG C ~ 65 DEG C, nanometer powder after must processing after cooling grinding, for subsequent use;
Step 2, the preparation of cyst material:
By trimeric cyanamide and formaldehyde mixing, at 70 DEG C of stirring reaction 30 ~ 50min, be down to normal temperature, obtain performed polymer, for subsequent use;
Step 3, nano material is adulterated:
Core material is placed heated and stirred in the water-bath with 50 DEG C and make its melting, get sodium salt that pH is the polystyrene-maleic acyl multipolymer of 7 or ammonium salt joins in core material, add step 1 gained nanometer powder, start high-shear emulsion machine with 3500 ~ 4000rpm, emulsification 20min ~ 30min, obtains the core material emulsion of composite nano materials;
Step 4, prepared by Nano capsule suspension:
Step 2 gained performed polymer is joined in step 3 gained core material emulsion, be placed in 40 DEG C of environment and at the uniform velocity stir with the speed of 200 ~ 300rpm, add the PH to 5 that acetic acid regulates emulsion, system temperature is slowly warming up to 70 DEG C from 40 DEG C in 60min simultaneously, 3 ~ 4h under Keep agitation, adjusting PH with 10% sodium carbonate solution is 7, after termination reaction, obtains the capsule suspension liquid of loaded with nano material;
Step 5, doped nano-material phase-change microcapsule powder is refined:
Step 4 gained microcapsule suspensions fast grade filter paper is filtered, and after repeatedly rinsing three times with dehydrated alcohol and distilled water, the drying in oven of 80 DEG C to constant weight, obtains the microscapsule powder of loaded with nano material.
2. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, is characterized in that, in step 1, alcoholic solvent is one in ethanol, methyl alcohol or Virahol or mixture.
3. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, it is characterized in that, in step 1, surface treatment agent is the one in 3-methacryloxypropyl trimethoxy silane, methyltrimethoxy silane, Union carbide A-162 octyltri-ethoxysilane, 3-mercaptopropyltriethoxysilane, trimethyl siloxanes, methyl trimethoxy oxygen radical siloxane, aminopropyl trimethoxysilane or vinyltrimethoxy silane.
4. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, it is characterized in that, in step 1, nano material is one in nano titanium oxide, nano stibium doped tin oxide, nano zine oxide, carbon nanotube, nano silicon, nanometer silicon carbide, nanometer iron powder, copper nanoparticle, nanometer aluminium powder, nano-nickel powder, nano-silver powder, nano-cerium oxide powder or nano lanthanum oxide powder or mixture.
5. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, is characterized in that, in step 1, the consumption of surface treatment agent solution is 1 ~ 10 times of nano material consumption.
6. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, is characterized in that, in step 2, the mass concentration of formaldehyde is 37%, and the mol ratio of trimeric cyanamide and formaldehyde is 1:1.6 ~ 2.5.
7. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, it is characterized in that, in step 3, core material is the one in bromotetradecane, bromohexadecane, bromo-octadecane, bromo eicosane, n-tetradecane, n-hexadecane, Octadecane or NSC 62789.
8. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, it is characterized in that, in step 3, the sodium salt of polystyrene-maleic acyl or the molecular weight of ammonium salt are 60,000 ~ 130,000, and the mass ratio of the sodium salt of polystyrene-maleic acyl or ammonium salt and core material is 1:5 ~ 10.
9. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, is characterized in that, in step 3, the consumption of nanometer powder is 0.5 ~ 20% of core material.
10. the preparation method of the phase-change microcapsule of a kind of doped with nanometer particle according to claim 1, is characterized in that, in step 4, the mass ratio of performed polymer and core material emulsion is 1:4 ~ 8.
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| CN113026136A (en) * | 2021-03-20 | 2021-06-25 | 浙江佳轩汽车用品有限公司 | Polyethylene fiber for automobile sun-proof protective sleeve and preparation method thereof |
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| CN113861942A (en) * | 2021-09-14 | 2021-12-31 | 中北大学 | Organic-microcapsule phase change material, preparation method thereof and application thereof in battery thermal management system |
| CN115318211A (en) * | 2022-09-08 | 2022-11-11 | 宁波大学 | Nanoparticle core material doped metal phase change microcapsule and preparation method thereof |
| CN115382475A (en) * | 2022-09-08 | 2022-11-25 | 宁波大学 | Nano particle wall material doped metal phase change microcapsule and preparation method thereof |
| CN115742483A (en) * | 2022-12-19 | 2023-03-07 | 山东雅满家生物质科技有限公司 | Composite floor and production method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009216A1 (en) * | 2006-07-14 | 2008-01-24 | Nano-Sports Technologies Ltd. | Preparation of composite nano/microcapsules comprising nanoparticles |
| CN101781395A (en) * | 2010-03-30 | 2010-07-21 | 上海交通大学 | Hard polyurethane adiabatic heat-insulation foam material and preparation method thereof |
| CN101824169A (en) * | 2010-01-19 | 2010-09-08 | 上海工程技术大学 | Natural rubber composite material with modified crystal whiskers 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 |
| CN104069783A (en) * | 2014-06-23 | 2014-10-01 | 东南大学 | Preparation method of carbon nanotube modified composite microcapsule |
-
2015
- 2015-05-18 CN CN201510253965.6A patent/CN104962240A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008009216A1 (en) * | 2006-07-14 | 2008-01-24 | Nano-Sports Technologies Ltd. | Preparation of composite nano/microcapsules comprising nanoparticles |
| CN101824169A (en) * | 2010-01-19 | 2010-09-08 | 上海工程技术大学 | Natural rubber composite material with modified crystal whiskers and preparation method thereof |
| CN101781395A (en) * | 2010-03-30 | 2010-07-21 | 上海交通大学 | Hard polyurethane adiabatic heat-insulation foam material 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 |
| CN104069783A (en) * | 2014-06-23 | 2014-10-01 | 东南大学 | Preparation method of carbon nanotube modified composite microcapsule |
Non-Patent Citations (5)
| Title |
|---|
| 吴忠元等: "硅烷偶联剂表面修饰四针状氧化锌晶须", 《应用化工》 * |
| 徐德彬等: "碳纳米管复合相变微胶囊的过冷性", 《天津工业大学学报》 * |
| 徐滨士主编: "《纳米表面工程》", 31 January 2004, 化学工业出版社 * |
| 揣成智等: "石蜡微胶囊的溶胶-凝胶法改性", 《应用化工》 * |
| 葛明桥等: "纤维用纳米二氧化硅粉体的表面改性及表征", 《合成纤维》 * |
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