CN109847663A - It is a kind of using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material - Google Patents
It is a kind of using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material Download PDFInfo
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Abstract
The present invention relates to a kind of using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, belongs to technical field of phase-change energy storage.This method, using n-capric acid-palmitinic acid binary of fatty acids eutectic mixture as phase-change microcapsule core material, is prepared using solvent evaporation method using polyvinyl chloride as phase-change microcapsule wall material, obtains low-temperature phase-change micro-capsule.It is of the invention using polyvinyl chloride as in the preparation method of the low-temperature phase-change micro-capsule of wall material, primary raw material used is from a wealth of sources, it is low in cost, and nonhazardous, therefore there is extraordinary environmental-protecting performance, tetrahydrofuran used can be recycled by condensation, water phase used is reusable after filtering out microcapsules, the waste and the pollution to environment for reducing resource.This method is easy to operate, environmental friendly, and required equipment requirement is low, is suitble to industrial mass production.Phase-change microcapsule function admirable of the invention, providing one kind for field of energy-saving technology can widely applied new type low temperature phase transformation microcapsules.
Description
Technical field
The present invention relates to a kind of using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, belongs to phase-change accumulation energy
Field of material technology.
Background technique
Phase change energy storage technology is a kind of to be absorbed using phase-change material in phase transformation and release latent heat to carry out thermal energy storage
Technology can solve thermal energy unmatched contradiction on time, intensity and place, be the important energy saving skill for improving efficiency of energy utilization
Art is applied to the fields such as Solar use, energy saving building material and aerospace.Phase when according to phase-change material phase transformation
Variation can be classified as solid-liquid phase change material and solid-solid phase change material, and solid-liquid phase change material is because phase transition temperature is wide, latent heat is big and valence
Lattice are low, are more widely applied.However, mobility of the solid-liquid phase change material in liquid phase will cause leakage, phase transformation material is seriously affected
The hot property of material, even results in environmental pollution.
For the leakage problems of solid-liquid phase change material, the solution that domestic and foreign scholars propose mainly includes that polymer is blended
Typing method, porous material absorption method and microcapsules package method.Wherein, microcapsules package method is because can effectively solve solid-liquid phase change material
Leakage, mutually separation and the problems such as corrosivity, protect core material not to be affected by the external environment, and bigger heat transfer can be provided for core material
Area and constant volume, it is considered to be optimal method.However, phase-change microcapsule is mainly with melamino-formaldehyde tree at present
Rouge, polyurethane, phenolic resin and Lauxite etc. are wall material, using situ aggregation method, interfacial polymerization and spray-on process system
Standby, complex process is with high costs, it is difficult to produce in batches, large-scale application is relatively difficult to achieve.
Summary of the invention
The purpose of the present invention is to propose to a kind of using polyvinyl chloride as low-temperature phase-change micro-capsule of wall material and preparation method thereof, with
Polyvinyl chloride is as phase-change microcapsule wall material, using n-capric acid-palmitinic acid binary of fatty acids eutectic mixture as phase-change microcapsule
Core material is prepared using solvent evaporation method, keeps raw material sources extensive, is prepared cheap.Machine is formed according to the cyst wall of wall material
System, finds preparation method easy to operate, environmental friendly, that actual production feasibility is strong, and finally obtaining can industrialized production and suitable
In widely applied new type low temperature phase transformation microcapsules.
It is proposed by the present invention using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, comprising the following steps:
(1) at 65-70 DEG C, by n-capric acid and palmitinic acid according to mass ratio 8.5:1.5 melting mixing after, stir 3-
7min, ultrasonic disperse 5-8min obtain binary of fatty acids eutectic mixture, as phase-change microcapsule core material；
(2) by phase-change microcapsule core material obtained in 2 parts of polyvinyl chloride and 1-3 parts of steps (1) in the condition being stirred continuously
Under be gradually dissolved into 40-70 parts of tetrahydrofurans, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 13-16 parts of sodium chloride are dissolved in 100 parts of distilled water, add 4-8 parts of gelatin,
It is stirred continuously to after being completely dissolved as water phase；
(4) oil obtained in 30 parts of steps (2) is mutually poured into reactor with water phase obtained in 90-100 parts of steps (3)
Mixing obtains homogeneous latex emulsion after stirring 1-2h under normal temperature conditions with the revolving speed of 700-1000r/min；
(5) reactor equipped with homogeneous latex emulsion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted
Temperature of reactor is saved to 55-58 DEG C, is continued stirring until until being flowed out in condensing unit without tetrahydrofuran；By residue in reactor
It is filtered, liquid will be filtered out and withdraw utilization, solid distilled water will be filtered out and ethyl alcohol cleans 2-3 times, be put into quiet in drier
48h is set, the low-temperature phase-change micro-capsule using polyvinyl chloride as wall material is obtained.
It is proposed by the present invention using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, its advantage is that:
1, of the invention using polyvinyl chloride as in the preparation method of the low-temperature phase-change micro-capsule of wall material, primary raw material used
For fatty acid, polyvinyl chloride, gelatin and sodium chloride, raw material sources are extensive, low in cost, and nonhazardous, therefore with very good
Environmental-protecting performance.
2, tetrahydrofuran used in the method for the present invention can be recycled by condensation, and water phase used is filtering out micro- glue
It is reusable after capsule, therefore the waste for greatly reducing resource and the pollution to environment.
3, preparation method of the invention, easy to operate, environmental friendly, required equipment requirement is low, is suitble to industrial mass
Production.
4, phase-change microcapsule function admirable prepared by the method for the present invention, providing one kind for field of energy-saving technology can be extensive
The new type low temperature phase transformation microcapsules of application.
Specific embodiment
It is proposed by the present invention using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, comprising the following steps:
(1) at 65-70 DEG C, by n-capric acid and palmitinic acid according to mass ratio 8.5:1.5 melting mixing after, stir 3-
7min, ultrasonic disperse 5-8min obtain binary of fatty acids eutectic mixture, as phase-change microcapsule core material；
(2) by phase-change microcapsule core material obtained in 2 parts of polyvinyl chloride and 1-3 parts of steps (1) in the condition being stirred continuously
Under be gradually dissolved into 40-70 parts of tetrahydrofurans, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 13-16 parts of sodium chloride are dissolved in 100 parts of distilled water, add 4-8 parts of gelatin,
It is stirred continuously to after being completely dissolved as water phase；
(4) oil obtained in 30 parts of steps (2) is mutually poured into reactor with water phase obtained in 90-100 parts of steps (3)
Mixing obtains homogeneous latex emulsion after stirring 1-2h under normal temperature conditions with the revolving speed of 700-1000r/min；
(5) reactor equipped with homogeneous latex emulsion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted
Temperature of reactor is saved to 55-58 DEG C, is continued stirring until until being flowed out in condensing unit without tetrahydrofuran；By residue in reactor
It is filtered, liquid will be filtered out and withdraw utilization, solid distilled water will be filtered out and ethyl alcohol cleans 2-3 times, be put into quiet in drier
48h is set, the low-temperature phase-change micro-capsule using polyvinyl chloride as wall material is obtained.
The embodiment of the method for the present invention introduced below:
Embodiment 1
(1) under the conditions of 65 DEG C, by 8.5g n-capric acid and 1.5g palmitinic acid melting mixing, 7min, ultrasonic disperse are stirred
5min obtains binary of fatty acids eutectic mixture, as phase-change microcapsule core material；
(2) 2g polyvinyl chloride and 2g binary of fatty acids eutectic mixture are gradually dissolved under conditions of being stirred continuously
In 60g tetrahydrofuran, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 26g parts of sodium chloride is dissolved in 171g distilled water, 9g gelatin is added, constantly stirs
It mixes to after being completely dissolved as water phase；
(4) oil obtained in step (2) is mutually poured into reactor with water phase obtained in step (3), in normal temperature condition
Under 1h is stirred with the revolving speed of 900r/min after, obtain homogeneous latex emulsion；
(5) reactor equipped with lotion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted anti-
It answers device temperature to 56 DEG C, continues stirring until until being flowed out in condensing unit without tetrahydrofuran；Residue in reactor is taken out
Filter will filter out liquid and withdraw utilization, will filter out solid distilled water and ethyl alcohol cleans 2 times, be put into drier and stand 48h, obtain
To using polyvinyl chloride as the low-temperature phase-change micro-capsule of wall material.
Phase-change microcapsule obtained by the present embodiment is that white is spherical, and for partial size between 40-60um, phase transition temperature is 21.46 DEG C,
Latent heat of phase change is 72.35J/g.
Embodiment 2
(1) under the conditions of 70 DEG C, by 17g n-capric acid and 3g palmitinic acid melting mixing, 3min, ultrasonic disperse 7min are stirred,
Binary of fatty acids eutectic mixture is obtained, as phase-change microcapsule core material；
(2) 4g polyvinyl chloride and 6g binary of fatty acids eutectic mixture are gradually dissolved under conditions of being stirred continuously
In 80g tetrahydrofuran, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 35g parts of sodium chloride is dissolved in 225g distilled water, add 15g gelatin, constantly
Stirring is used as water phase to after being completely dissolved；
(4) oil obtained in step (2) is mutually poured into reactor with water phase obtained in step (3), in normal temperature condition
Under 2h is stirred with the revolving speed of 800r/min after, obtain homogeneous latex emulsion；
(5) reactor equipped with lotion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted anti-
It answers device temperature to 58 DEG C, continues stirring until until being flowed out in condensing unit without tetrahydrofuran；Residue in reactor is taken out
Filter will filter out liquid and withdraw utilization, will filter out solid distilled water and ethyl alcohol cleans 3 times, be put into drier and stand 48h, obtain
To using polyvinyl chloride as the low-temperature phase-change micro-capsule of wall material.
Phase-change microcapsule obtained by the present embodiment is that white is spherical, and for partial size between 50-90um, phase transition temperature is 22.78 DEG C,
Latent heat of phase change is 82.69J/g.
Embodiment 3
(1) under the conditions of 68 DEG C, by 8.5g n-capric acid and 1.5g palmitinic acid melting mixing, 5min, ultrasonic disperse are stirred
6min obtains binary of fatty acids eutectic mixture, as phase-change microcapsule core material；
(2) 4g polyvinyl chloride and 2g binary of fatty acids eutectic mixture are gradually dissolved under conditions of being stirred continuously
In 100g tetrahydrofuran, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 42g parts of sodium chloride is dissolved in 282g distilled water, add 18g gelatin, constantly
Stirring is used as water phase to after being completely dissolved；
(4) oil obtained in step (2) is mutually poured into reactor with water phase obtained in step (3), in normal temperature condition
Under 1h is stirred with the revolving speed of 700r/min after, obtain homogeneous latex emulsion；
(5) reactor equipped with lotion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted anti-
It answers device temperature to 57 DEG C, continues stirring until until being flowed out in condensing unit without tetrahydrofuran；Residue in reactor is taken out
Filter will filter out liquid and withdraw utilization, will filter out solid distilled water and ethyl alcohol cleans 2 times, be put into drier and stand 48h, obtain
To using polyvinyl chloride as the low-temperature phase-change micro-capsule of wall material.
Phase-change microcapsule obtained by the present embodiment is that white is spherical, and partial size is between 60-110um, phase transition temperature 20.13
DEG C, latent heat of phase change 47.82J/g.
Claims (1)
1. a kind of using polyvinyl chloride as the preparation method of the low-temperature phase-change micro-capsule of wall material, it is characterised in that the preparation method includes
Following steps:
(1) at 65-70 DEG C, by n-capric acid and palmitinic acid according to mass ratio 8.5:1.5 melting mixing after, stir 3-7min, surpass
Sound disperses 5-8min, binary of fatty acids eutectic mixture is obtained, as phase-change microcapsule core material；
(2) by phase-change microcapsule core material obtained in 2 parts of polyvinyl chloride and 1-3 parts of steps (1) under conditions of being stirred continuously by
It is gradually dissolved into 40-70 parts of tetrahydrofurans, ultrasonic disperse is uniformly afterwards as oily phase；
(3) under the conditions of 60 DEG C, first 13-16 parts of sodium chloride are dissolved in 100 parts of distilled water, add 4-8 parts of gelatin, constantly
Stirring is used as water phase to after being completely dissolved；
(4) oil obtained in 30 parts of steps (2) is mutually poured into reactor and is mixed with water phase obtained in 90-100 parts of steps (3)
It closes, after stirring 1-2h under normal temperature conditions with the revolving speed of 700-1000r/min, obtains homogeneous latex emulsion；
(5) reactor equipped with homogeneous latex emulsion is connected to condensing unit, first adjusting speed of agitator to 400r/min, then adjusted anti-
It answers device temperature to 55-58 DEG C, continues stirring until until being flowed out in condensing unit without tetrahydrofuran；Residue in reactor is carried out
It filters, liquid will be filtered out and withdraw utilization, solid distilled water will be filtered out and ethyl alcohol cleans 2-3 times, be put into drier and stand
48h obtains the low-temperature phase-change micro-capsule using polyvinyl chloride as wall material.
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| CN110408143A (en) * | 2019-06-27 | 2019-11-05 | 湖北英特吉新能源科技有限公司 | A kind of foaming figuration composite phase-changing material and preparation method thereof |
| CN113528093A (en) * | 2021-06-18 | 2021-10-22 | 东南大学 | Yeast cell wall-coated phase-change material microcapsule and preparation method and application thereof |
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Cited By (2)
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| CN110408143A (en) * | 2019-06-27 | 2019-11-05 | 湖北英特吉新能源科技有限公司 | A kind of foaming figuration composite phase-changing material and preparation method thereof |
| CN113528093A (en) * | 2021-06-18 | 2021-10-22 | 东南大学 | Yeast cell wall-coated phase-change material microcapsule and preparation method and application thereof |
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