CN107020054A - A kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes - Google Patents
A kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes Download PDFInfo
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- CN107020054A CN107020054A CN201710090229.2A CN201710090229A CN107020054A CN 107020054 A CN107020054 A CN 107020054A CN 201710090229 A CN201710090229 A CN 201710090229A CN 107020054 A CN107020054 A CN 107020054A
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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
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- C—CHEMISTRY; METALLURGY
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- 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
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The invention provides a kind of preparation method of the phase-change microcapsule with high thermal conductivity coefficient and uniform particle sizes.Using metallic particles doping and drop microflow control technique, a step carries out emulsification and the capsulating process of phase-change material in micro-fluidic chip.The metal nanoparticle of phase-change material doping high thermal conductivity coefficient in capsule, so that the thermal conductivity factor of capsule has obtained effective raising, the heat transfer property of phase-change microcapsule is enhanced, while the latent heat of phase change reduction of capsule in itself is considerably less, the practical value of capsule is added；The present invention prepares phase-change material microemulsion using drop microflow control technique, and the emulsion process of drop is accurately controlled using high-precision syringe pump, the narrow monodisperse phase-change material microemulsion of particle diameter distribution is obtained.Preparation process has equipment simple, easily operation, and waste of raw materials is few, it is easy to controls the advantages of particle diameter, noiseless pollution, low energy consumption, is suitable for scientific research and the popularization and application of industrial production phase-change microcapsule.
Description
Technical field
The invention belongs to phase-change microcapsule technical field of material.The high heat conduction phase transformation of specifically related to a kind of uniform particle sizes
The preparation method of microcapsules.
Background technology
Phase-change microcapsule (encaps μ late phase change materials, MEPCMS) refers to that inside is surrounded by phase
Become the capsule of the micron size of material.Phase-change microcapsule is generally divided into two parts：The capsule-core and one of one phase-change material composition
Individual macromolecule or mineral shell are referred to as cyst wall.Capsule typically all has unified regular or irregular profile, capsule
Profile is generally dependent on the shape of capsule-core and the forming process of shell.Capsule-core is by one or more kinds of material compositions.Cyst wall is usual
The formation such as high polymer material or inorganic matter for using, and cyst wall has individual layer and point of multilayer.The encapsulated of phase-change material makes
Solid-liquid change can constantly be occurred by obtaining phase-change material (PCM) in script application process realizes persistent solid-state, not only remains
The physical property of PCM scripts, while overcome that traditional phase-change material has is unstable.Additionally by the special wall material of use
Be modified technique, phase-change microcapsule can also overcome the capacity of heat transmission poor, it is inflammable it is volatile wait conventional phase change material have lack
Point.Phase-change microcapsule is widely used in the neck such as accumulation of heat temperature control material, building energy conservation, low-grade energy utilization, Aero-Space, military affairs
Domain.The research of phase-change microcapsule originates in 20 century 70s：Ground earliest by the scientist of the states such as Germany, South Korea, Japan
Study carefully, Chinese phase-change microcapsule technology is started late, be probably to add the micro- glue of phase transformation from 1990s Chinese Scientists
The research ranks of capsule simultaneously achieve certain achievement.At present, in states such as the U.S., Japan, Germany, phase-change microcapsule technology is realized
Preliminary industrialization, German BASF AG is presently the most the company for being successfully prepared and selling phase-change microcapsule.
The preparation method of general microcapsules has following several：Chemical method：Situ aggregation method, interfacial polymerization, orifice-solidification
Bath method and electroless plating method etc.；Physical-chemical process：Aqueous phase separation method, oil-phase separating method, dry bath method, fusing scattered condensation method, powder
Last bed process and capsule-core exchange process etc.；Physical method：It is air suspension, spray drying process, spray chilling method, spray cooling, true
Empty evaporation deposition method, supercritical fluid method and electrostatical binding method etc..Although the method for preparing microcapsules at present is numerous, mainly
There are situ aggregation method, interfacial polymerization, complex coacervation and spray drying process for preparing the method for phase-change microcapsule.These are prepared
The general all operating process of the method for phase-change microcapsule are complicated, and the capsule grain diameter distribution prepared is wide, and particle size is difficult to control,
The capsule heat conductivility prepared is poor so that the use of phase-change microcapsule is restricted.
Microflow control technique develops gradually maturation in drop preparation field in recent years, can be prepared using microflow control technique many
The single dispersing drop of material is planted, can also be in droplet surface film forming by the integrated chemical reactive moieties on micro-fluidic chip.It is single
The size of dispersant liquid drop can realize accurate control by changing continuous phase and dispersed phase inlet velocity.Micro-fluidic core is used at present
The phase-change microcapsule that piece prepares the doping high heat conducting nano particle of uniform particle sizes is rarely reported.
The content of the invention
The phase-change microcapsule particle diameter distribution prepared for existing preparation method is big, and the shortcoming of heat transfer property difference, the present invention is carried
The particle diameter of doping high-termal conductivity titanium dioxide nanoparticle is gone out to be prepared with homemade quartz capillary coaxial flow micro-fluidic chip
The phase-change microcapsule of uniform, controllable.
The technical problem to be solved in the present invention is to provide a kind of system of the controllable high-termal conductivity phase-change microcapsule of uniform particle sizes
Preparation Method.
The preparation method of the high heat conduction phase-change microcapsule of a kind of uniform particle sizes of the present invention, it is characterised in that step includes：
(1) capillary glass tube micro-fluidic chip is made:It it is 500-1000 microns from external diameter, internal diameter is 100-500 microns
Capillary glass tube 2, interior length of side 500-1000 microns, 1, outer length of side 1000-1500 microns of square glass capillary；Make
It is sharp mouth to be drawn a circular capillaries one end with wire drawing machine, and sharp mouth internal diameter is 10-100 microns, by another circular capillary
The wire drawing of pipe one end into internal diameter be 50-500 microns of necking；By the taper end of 2 circular capillaries wire drawings from square capillary two
End alignment insertion, both distance between two tips are 100-500 microns, and both axis are on the same line；By the capillary assembled
It is placed on transparent slide, the interface of sharp mouth capillary and square capillary is tipped upside down on using conical centrifuge tube, forms one
Individual liquid-accumulating trough.Seal up circular capillaries, conical centrifuge tube and square intercapillary gap respectively using epoxide-resin glue；
In tap web centrifuge tube tip punching insertion conduit, and seal up using epoxy resin glue the gap between conduit and centrifuge tube；
(2) for the coaxial flow pattern micro-fluidic chip that uses, by the phase-change material of the high heat conducting nano particle of pre-coated and
The mixed liquor of toluene di-isocyanate(TDI) (TDI) is as dispersed phase, a certain proportion of surfactant and TEPA (TEPA)
The aqueous solution be used as continuous phase.
(3) by two precise injection pumps, different fluid injection flow velocitys are adjusted, by phase-change material, water each leads into microchannel
Inner circular capillary and external square capillary, ultimately form phase-change material microemulsion.
(4) microemulsion flowed out from microchip outlet section is collected, insulation is placed 10 hours in 45 DEG C of insulating boxs；
(5) microemulsion that reaction is obtained in step (4) is filtered, using deionized water cleaning for several times, freeze-drying,
It can obtain the uniform high heat conduction phase-change microcapsule of target grain size.
The high heat conduction phase-change microcapsule of the uniform particle sizes is by linear paraffin or linear paraffin halides doping quality point
Number is constituted for high heat conducting nano particles such as 1%-5% metal, metal oxide, graphenes as core and polyureas as wall material
, its size is 30-500 microns, and phase-change microcapsule particle diameter deviation is less than 4 microns, the main phase transformation capsule proportion for preparing size
More than 50%.Core content is 70-90%.
In step (2), it is dispersed phase that the phase-change material being passed through from the capillary with sharp mouth, which is referred to as, is passed through from liquid-accumulating trough
Water be referred to as continuous phase.
Step (1) makes circular capillaries its external diameter that microchip uses and is slightly less than the square capillary length of side；Microchip enters
Mouthful be step (1) in cuspidated circular capillaries and tapered capillaries liquid-accumulating trough, export as the circular capillary with necking
Pipe；Necking internal diameter and the internal diameter ratio at tip are more than 1 and are less than 10.
Phase-change material selected by step (2) is linear paraffin or linear paraffin halides, preferably heptadecane, and high heat conduction is received
Rice grain is the rutile-type titanium dioxide of metal, metal oxide, graphene, preferably titanium dioxide, more preferably 50 nanometers of particle diameter
Titanium；The preferred neopelex of surfactant (SDBS).
Preferably titanium dioxide is mixed with heptadecane fused solution in step (2), makes titanium dioxide uniform using ultrasonic disperse
It is dispersed in heptadecane.
The mass fraction that contained TDI mass fraction is contained TEPA in 2%-5%, water in phase-change material is 4%-6%.
The titania-doped mass fraction of step (2) described phase-change material is 0.1%-5%, and density is 0.78-
0.88g·cm-3.Thermal conductivity factor is 0.22-0.40wm-1K-1.
Step (2) described solution density is 0.990-1.000gcm-3.Microemulsion preparation temperature is 20-30 DEG C.
Coaxial flow pattern micro-fluidic chip, 9 internal diameters of circular capillaries tip are 30-50um, the internal diameter of circular capillaries 4 and 7
Length of side 500um in 300um, external diameter 500um, square capillary.Dispersed phase and continuous phase velocity ratio are adjusted between 1-10.
In the preparation method of the high heat conduction phase-change microcapsule of above-mentioned uniform particle sizes, further preferred implementation is：
The mass fraction of titanium dioxide is 2%-3%, TDI mass concentration in the doping phase transiting material that step (1) is used
It is 5% for 2%, TEPA mass fraction.The mass fraction of neopelex is 4%.
Step (4) temperature for preparing double emulsions is 25 DEG C.The flow velocity of continuous phase and dispersed phase is respectively 10-15 μ
ml·min-1、20-30μ ml·min-1。
The present invention with homemade capillary glass tube coaxial flow micro-fluidic chip is experimental bench, by adjusting dispersed phase and continuous
The velocity ratio of phase controls the particle size of phase-change microcapsule.The heat transfer of microcapsules is controlled by adjusting the doping ratio of nano particle
Performance, the solidification process of capsule-wall is controlled by the ratio and concentration and reaction time that adjust polymerized monomer.
The beneficial effects of the invention are as follows the metal oxide nanoparticles that high-termal conductivity is doped with inside microcapsules so that phase
Become heat transfer coefficient of the microcapsules in phase transition process to be effectively improved, improve energy storage efficiency.Phase transformation can be realized simultaneously
Microcapsule size is controllable.The preparation method equipment is simple, and preparation process is noiseless, is suitable for laboratory scientific research and plant produced should
With.
Brief description of the drawings
The micro-fluidic chip design drawing that Fig. 1 uses for the present invention
Specific implementation method
The technical problem to be solved in the present invention is to provide a kind of system of the controllable high-termal conductivity phase-change microcapsule of uniform particle sizes
Preparation Method.Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example is applied, the scope of protection of the invention is belonged to.
The preparation method of the uniform grading high heat conduction phase-change microcapsule of the present invention, in turn includes the following steps：
(1) it refer to shown in Fig. 1, make capillary glass tube micro-fluidic chip:It is 500-1000 microns, internal diameter from external diameter
For 100-500 microns of capillary glass tube 2, interior length of side 500-1000 microns, outer length of side 1000-1500 microns of square glass
1, capillary；It is sharp mouth 9 to be drawn the one end of circular capillaries 4 using wire drawing machine, and the sharp internal diameter of mouth 9 is 10-100 microns, will
Another one end wire drawing of circular capillaries 7 into internal diameter be 50-500 microns of necking 10；By the thin of 2 circular capillaries wire drawings
End is aligned from the square two ends of capillary 11 and inserted, and both distance between two tips are 100-500 microns, and both axis are in same straight line
On；The capillary assembled is placed on transparent slide 6, sharp mouth capillary is tipped upside down on and square using conical centrifuge tube 3
The interface of capillary, forms a liquid-accumulating trough.Circular capillaries, conical centrifuge are sealed up respectively using epoxide-resin glue 5 and 8
Pipe and square intercapillary gap；In tap web centrifuge tube tip punching insertion conduit 1, and use epoxide-resin glue water-stop
The firmly gap 2 between conduit and centrifuge tube；
(2) for the coaxial flow pattern micro-fluidic chip that uses, by the phase-change material of the blended metal oxide of pre-coated and
TDI mixed liquor is used as continuous phase as dispersed phase, the aqueous solution of a certain proportion of surfactant and TEPA.
(3) heat conduction system of the phase-change material of measure (1) described doping metals or metal oxide under different doping ratios
Number and density, determine optimal doping ratio.
(4) density of (1) described dispersed phase phase-change material and the continuous phase aqueous solution at different temperatures is determined respectively, it is determined that
The preparation of phase-change material microemulsion and reaction temperature.
(5) by two precise injection pumps, different fluid injection flow velocitys are adjusted, by phase-change material, water each leads into microchannel
Inner circular capillary and external square capillary, ultimately form phase-change material microemulsion.
(6) microemulsion flowed out from microchip outlet section is collected, insulation is placed 10 hours in 45 DEG C of insulating boxs；
(7) microemulsion that reaction is obtained in step (5) is filtered, using deionized water cleaning for several times, freeze-drying,
It can obtain the uniform high heat conduction phase-change microcapsule of target grain size.
Step (1) makes circular capillaries its external diameter that microchip uses and is slightly less than the square capillary length of side；Microchip enters
Mouthful be step (1) in cuspidated circular capillaries and tapered capillaries liquid-accumulating trough, export as the circular capillary with necking
Pipe；Necking internal diameter and the internal diameter ratio at tip are more than 1 and are less than 10.
Phase-change material selected by step (2) is water insoluble heptadecane, and high heat conducting nano particle is titanium dioxide, will
Titanium dioxide is mixed with heptadecane fused solution, titanium dioxide is dispersed in heptadecane using ultrasonic disperse.Phase-change material
In contained TDI mass fraction be contained TEPA in 2%-5%, water mass fraction be 4%-6%.
The titania-doped mass fraction of step (2) described phase-change material is 0.1%-5%, and density is 0.78-
0.88g·cm-3.Thermal conductivity factor is 0.22-0.40wm-1·K-1。
Step (4) described solution density is 0.990-1.000gcm-3.Microemulsion preparation temperature is 20-30 DEG C.
The coaxial flow pattern micro-fluidic chip of step (5), 9 internal diameters of circular capillaries tip are 30-50um, circular capillaries 4 and 7
Length of side 500um in internal diameter 300um, external diameter 500um, square capillary.Dispersed phase and continuous phase velocity ratio are adjusted between 1-10.
In the preparation method of the high heat conduction phase-change microcapsule of above-mentioned uniform particle sizes, further preferred implementation is：
The mass fraction of titanium dioxide is 2%-3%, TDI mass concentration in the doping phase transiting material that step (1) is used
It is 5% for 2%, TEPA mass fraction.The mass fraction of neopelex is 4%.
Step (4) temperature for preparing double emulsions is 25 DEG C.The flow velocity of continuous phase and dispersed phase is divided into 10-15 μm of l
min-1、20-30μ ml·min-1。
Embodiment 1
(1) 4ml heptadecane mixed liquors are taken with 5ml syringes, the 15ml aqueous solution is taken with 20ml syringes, syringe is fixed
On precise injection pump, by Teflon conduit respectively with being led in the sharp mouth circular capillaries and tap web centrifuge tube of micro-fluidic chip
Pipe is connected.
(2) it is respectively 10 μm of lmin to adjust coaxial flow microchip continuous phase and dispersed phase flow velocity-1With 20 μm of lmin-1。
Continuous phase is first passed through, then is passed through dispersed phase.
(3) microemulsion flowed out from microchip outlet section is collected, insulation is placed 10 hours and carries out glue in 45 DEG C of insulating boxs
The curing reaction of capsule cyst wall.
(4) suspension after the completion of solidification is filtered, using deionized water cleaning for several times, freeze-drying obtains grain
Footpath is 100 μm, and polydispersity is less than the phase-change microcapsule of 3% doped nano titanium dioxide.
Embodiment 2
Step (1), (3) are with embodiment 1.
It is respectively 15 μm of lmin that step (2), which saves coaxial flow microchip continuous phase and dispersed phase flow velocity,-1With 20 μm of lmin-1.Continuous phase is first passed through, then is passed through dispersed phase.
Step (4) is with embodiment 1, but it is 150 μm to obtain particle diameter, and polydispersity is less than 3% dopen Nano titanium dioxide
The phase-change microcapsule of titanium.
Embodiment 3
Step (1) takes 2ml paraffin and titanium dioxide TDI mixed liquor with 5ml syringes, and 15ml is taken with 20ml syringes
The mixed liquor of water, neopelex and TEPA, connects dispersed phase and the interface of continuous phase respectively.
Step (2), (3), (4) are with embodiment 1.
Claims (7)
1. the preparation method of the high heat conduction phase-change microcapsule of a kind of uniform particle sizes, it is characterised in that preparation method step includes：
(1) capillary glass tube micro-fluidic chip is made:It it is 500-1000 microns from external diameter, internal diameter is 100-500 microns of glass
2, glass capillary, interior length of side 500-1000 microns, 1, outer length of side 1000-1500 microns of square glass capillary；Use drawing
It is sharp mouth that silk machine, which draws a circular capillaries one end, and sharp mouth internal diameter is 10-100 microns, by another circular capillaries one
Wire drawing is held into the necking that internal diameter is 50-500 microns；By the taper end of 2 circular capillaries wire drawings from square capillary two ends pair
Quasi- insertion, both distance between two tips are 100-500 microns, and both axis are on the same line；The capillary assembled is placed
On transparent slide, the interface of sharp mouth capillary and square capillary is tipped upside down on using conical centrifuge tube, a storage is formed
Liquid bath.Seal up circular capillaries, conical centrifuge tube and square intercapillary gap respectively using epoxide-resin glue；In cone
Heart centrifuge tube tip punching insertion conduit, and seal up using epoxy resin glue the gap between conduit and centrifuge tube；
(2) for the coaxial flow pattern micro-fluidic chip used, by the phase-change material and toluene of the high heat conducting nano particle of pre-coated
The mixed liquor of diisocyanate (TDI) is used as dispersed phase, the water of a certain proportion of surfactant and TEPA (TEPA)
Solution is used as continuous phase.
(3) by two precise injection pumps, different fluid injection flow velocitys are adjusted, by phase-change material, water each leads into the interior of microchannel
Portion's circular capillaries and external square capillary, ultimately form phase-change material microemulsion.
(4) microemulsion flowed out from microchip outlet section is collected, insulation is placed 10 hours in 45 DEG C of insulating boxs；
(5) microemulsion that reaction is obtained in step (4) is filtered, using deionized water cleaning for several times, freeze-drying, you can
Obtain the uniform high heat conduction phase-change microcapsule of target grain size.
2. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 1, it is characterised in that：
In step (2), it is dispersed phase that the phase-change material being passed through from the capillary with sharp mouth, which is referred to as, and the water being passed through from liquid-accumulating trough is referred to as
Continuous phase.
3. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 1, it is characterised in that：
Step (1) makes circular capillaries its external diameter that microchip uses and is slightly less than the square capillary length of side；Microchip entrance is step
(1) with cuspidated circular capillaries and tapered capillaries liquid-accumulating trough in, export as the circular capillaries with necking；In necking
The internal diameter ratio at footpath and tip is more than 1 and is less than 10.
4. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 1, it is characterised in that：
Phase-change material selected by step (2) is linear paraffin or linear paraffin halides, preferably heptadecane, high heat conducting nano
Grain is the rutile titanium dioxide of metal, metal oxide, graphene, preferably titanium dioxide, more preferably 50 nanometers of particle diameter；Table
The preferred neopelex of face activating agent (SDBS)；TDI mass fractions are 2%-5%, TEPA mass fractions in step (4)
For 4%-8%.
5. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 4, it is characterised in that：
Phase-change material selected by step (2) is preferred heptadecane, and the preferred titanium dioxide of high heat conducting nano particle, more preferably particle diameter 50 are received
The rutile titanium dioxide of rice；The preferred neopelex of surfactant (SDBS).
6. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 1, it is characterised in that：
The flow velocity of continuous phase and dispersed phase is respectively 10-15 μm of lmin-1,20-30 μm lmin-1.
7. a kind of preparation method of the high heat conduction phase-change microcapsule of uniform particle sizes according to claim 1, it is characterised in that：
The high heat conduction phase-change microcapsule of the uniform particle sizes is to adulterate mass fraction by linear paraffin or linear paraffin halides for 1%-
The high heat conducting nano such as 5% metal, metal oxide, graphene particle is constituted as core and polyureas as wall material, its chi
Very little is 30-500 microns, and phase-change microcapsule particle diameter deviation is less than 4 microns, and the main phase transformation capsule proportion for preparing size is more than
50%.Core content is 70-90%.
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| CN108378417A (en) * | 2018-04-20 | 2018-08-10 | 广西中烟工业有限责任公司 | A kind of preparation method of the quick-fried pearl of water-soluble core material based on milli fluidics |
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| CN110479191A (en) * | 2019-08-27 | 2019-11-22 | 广东工业大学 | A kind of liquid metal microballoon and the preparation method and application thereof |
| CN110694704A (en) * | 2019-09-26 | 2020-01-17 | 安徽省昂普拓迈生物科技有限责任公司 | Portable quick micro-droplet generator |
| CN110694704B (en) * | 2019-09-26 | 2021-10-12 | 安徽省昂普拓迈生物科技有限责任公司 | Portable quick micro-droplet generator |
| CN114054763A (en) * | 2020-07-29 | 2022-02-18 | 中国科学院理化技术研究所 | Multi-shape liquid metal particle and preparation method thereof |
| CN114054763B (en) * | 2020-07-29 | 2024-02-27 | 中国科学院理化技术研究所 | Multi-shape liquid metal particle and preparation method thereof |
| CN112546978A (en) * | 2020-11-23 | 2021-03-26 | 广东工业大学 | Multifunctional phase change microcapsule and preparation method thereof |
| CN114410281A (en) * | 2022-02-08 | 2022-04-29 | 广东工业大学 | High-cycle inorganic hydrated salt phase change nanocapsule and preparation method and application thereof |
| CN114410281B (en) * | 2022-02-08 | 2023-10-03 | 广东工业大学 | High-circulation inorganic hydrated salt phase-change nanocapsule, and preparation method and application thereof |
| CN114797699A (en) * | 2022-04-22 | 2022-07-29 | 广东工业大学 | Method for eliminating supercooling degree of paraffin phase change microcapsule and causing no loss of phase change enthalpy, prepared phase change microcapsule and application thereof |
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