CN103059814A - Phase change material - Google Patents
Phase change material Download PDFInfo
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- CN103059814A CN103059814A CN2011103254858A CN201110325485A CN103059814A CN 103059814 A CN103059814 A CN 103059814A CN 2011103254858 A CN2011103254858 A CN 2011103254858A CN 201110325485 A CN201110325485 A CN 201110325485A CN 103059814 A CN103059814 A CN 103059814A
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Abstract
The invention provides a phase change material 4-(4-dimethyl amino styryl) methylpyridine trifluoro sulfonate. The material is subjected to reversible phase change at the temperature of about 320K; and the latent heat in the phase change process is more than 2000J/mol. The chemical formula of the compound is C17H19N2O3F3S; the compound belongs to the monoclinic system at normal temperature, and the space group is P21/c; and the space group also is P21/c at the temperature of higher than 320K, just the cell parameter changes significantly. The phase change process of the material is reversible; the material can be recycled for several times and has latent application value in the aspects of energy storage device, energy saving system and the like; in addition, the dielectric property of the material in the phase change process changes in a step type; and the material can be used as the candidate material in the fields of controllable dielectric capacitor, controllable dielectric grating and the like.
Description
Technical field
The present invention relates to a kind of phase change material, belong to field of functional materials, specially refer to 4-(4-dimethylamino styryl) picoline three fluoro sulfonates as phase change material and application thereof.
Background technology
Phase change material is the important materials that realizes energy source optimization utilization and energy-saving and emission-reduction, in the process that material undergoes phase transition, can absorb heat from environment (cold) or to environment heat release (cold), thereby realize energy storage, release can and the purpose of adjusting energy demand.Utilize the latent heat of phase change material to carry out storage or the release of energy, can produce the device of various high-energy utilization ratios; Simultaneously, in the transformation temperature scope, show unique electrical properties, thermal property according to phase change material, can design various multi-functional devices, such as high-k electric capacity, controlled dielectric grating and optical waveguides circulator etc.Therefore, this class material has huge application prospect in fields such as sun power utilization, waste heat waste heat recovery, intelligent automatic air-conditioning and construction thing, phase-changing energy-storing type air-conditioning, electrical equipment constant temperature, and along with the progressively development of technology, the range of application of materials constantly enlarges.
Wherein, transformation temperature phase change material of (30～50 ℃) more than room temperature has very important purposes, especially in the daily lifes such as building, automobile, such as (Zhang Xiong such as heat insulation coating, heat insulation phase transformation energy-saving materials, Zhang Yongjuan compiles, " modern architectural functions material ", Chemical Industry Press, in August, 2009).But existing material category in this this phase transition temperature interval is less, the shortcomings such as that some materials exist is little such as latent heat of phase change, stability is poor, production cost is high even corrodibility is strong are so that its application in fields such as building and lives has been subject to greatly restriction.Therefore, synthetic and preparation latent heat in phase transition process is large, stability height, low production cost, nontoxic non-corrosive phase change material have important practical value.
Summary of the invention
The object of the present invention is to provide that a kind of synthetic method is simple, with low cost, reaction conditions is gentle, stable higher organic phase change material and the application thereof of calorifics.
The invention provides the preparation method of a kind of phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates:
(1) be to be dissolved in an amount of methyl alcohol at 1: 1: 1 in molar ratio with 4-picoline, methyl iodide and 4-dimethylamino benzaldehyde, stir and slowly be warming up to 65～70 ℃, carry out back flow reaction 10～12h take piperidines as catalyzer, solution colour is by the light yellow scarlet that gradually becomes, after crystallisation by cooling, filtration, oven dry, obtain 4-(4-dimethylamino styryl) picoline iodide;
(2) temperature is under 50 ℃ the condition, in the methyl alcohol of 50～75mL, be to carry out ion exchange reaction at 1: 1 in molar ratio with gained 4-(4-dimethylamino styryl) picoline iodide and three fluosulfonic acid silver, after removing by filter precipitation, solution through leave standstill, cooling, crystallization, can get target product.
The skeleton symbol of a kind of organic phase change material 4-provided by the present invention (4-dimethylamino styryl) picoline three fluoro sulfonates is as follows:
X-ray single crystal diffraction test result shows: the chemical formula of this compound is C
17H
19N
2O
3F
3S belongs to oblique system under the room temperature, and spacer is P2
1/ c, unit cell parameters is a=17.508 (5), b=7.607 (2), c=13.533 (4)
α=90.0 °, β=93.712 (6) °, γ=90.0 °, Z=4, V=1798.4 (10)
Differential heat scan calorimeter (DSC) is measured transformation temperature and the enthalpy of phase change of material, the result shows: material underwent phase transition when temperature was 47 ℃, and the transformation temperature scope is about 47～55 ℃, and the latent heat in the phase transition process is greater than 2000J/mol, phase transition process is reversible, can repeatedly recycle.
When temperature is 70 ℃, record compound for also being oblique system, spacer is P2
1/ c, but considerable change has occured in unit cell parameters, for: a=7.190 (9)
B=7.698 (10)
C=34.08 (4)
α=γ=90.0 °, β=90.05 (4) °, Z=4, V=1886 (4)
Adopt the dielectric properties of bridge method test material in the transformation temperature scope, the result shows: the relative permittivity of material changes when temperature is 47 ℃, and the relative permittivity under the hot conditions is 1.5～2 times of relevant parameter under the cold condition approximately.
Description of drawings
The transformation temperature curve of Fig. 1, phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates.
The heat decomposition curve of Fig. 2, phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates.
The relative permittivity temperature variant curve of Fig. 3, phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates on (001) direction.
Below in conjunction with the drawings and specific embodiments the present invention is further described.
Embodiment
Embodiment 1: the preparation of phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates
With 4-picoline (5 * 10
-3Mol), methyl iodide (5 * 10
-3Mol) and 4-dimethylamino benzaldehyde (5 * 10
-3Mol) be dissolved in 50～100mL methyl alcohol, stir and slowly be warming up to 65～70 ° ℃, add 3～5mL piperidines and carry out back flow reaction 10～12h as catalyzer, solution colour is by the faint yellow scarlet that gradually becomes, solution is after crystallisation by cooling, filtration, oven dry, obtain 4-(4-dimethylamino styryl) picoline iodide, productive rate is 84.2%.
Temperature is under 50 ℃ the condition, with 2.5 * 10
-3Mol 4-(4-dimethylamino styryl) picoline iodide and 2.5～3.0 * 10
-3Mol three fluosulfonic acid silver react about 2h in 25～40mL methyl alcohol, remove by filter precipitation, solution through leaving standstill, cooling, crystallization get red needle-like or block target product, i.e. 4-(4-dimethylamino styryl) picoline three fluoro sulfonates, productive rate is 90.4%.
Case study on implementation 2:
As implement case 1 preparation 4-(4-dimethylamino styryl) picoline iodide;
Under 50 ℃ reaction conditions, 0.01mol 4-(4-dimethylamino styryl) picoline iodide are dissolved in the 75mL methyl alcohol, 0.05mol trifluoro sodium sulfonate is dissolved in the 40mL water, the about 48h of both mix and blend ion exchange reactions, solution is through leaving standstill, cool off, and in methyl alcohol recrystallization, get red needle-like target product, be 4-(4-dimethylamino styryl) picoline three fluoro sulfonates, productive rate is about 50.3%.The application of case study on implementation 3 phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates aspect energy storage
Case study on implementation 1 resulting phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates are carried out performance test, the DSC curve as shown in Figure 1, its phase change characteristics is: in the temperature-rise period, material absorbs heat in 47～55 ℃ temperature range and undergoes phase transition, and the latent heat that absorbs is greater than 2000J/mol; In the temperature-fall period, the material generation reversible transformation that releases energy.Therefore, in above-mentioned transformation temperature scope, this phase change material can be used as the candidate material of heat accumulation.
In addition, thermal analysis curve shown in Figure 2 shows: case study on implementation 1 resulting phase change material did not decompose before 274 ℃, had good thermal stability.
The application of case study on implementation 4 phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates aspect dielectric devices
Adopt bridge method that case study on implementation 1 resulting phase change material 4-(4-dimethylamino styryl) picoline three fluoro sulfonates are carried out the dielectric properties test, its along the relative permittivity variation with temperature curve of (001) direction as shown in Figure 3, the result shows:
In the temperature-rise period, the relative permittivity of material occurs significantly to change near 47 ℃, and during such as frequency f=1KHz, relative permittivity increases to 53.8 fast by 36.2, is about original 1.5 times.This variation has confirmed further that not only material undergoes phase transition near this temperature, and shows that material has potential using value in fields such as controlled dielectric electric capacity, controlled dielectric gratings.
Claims (4)
1. phase change material, this materials chemistry formula is C
17H
19N
2O
3F
3S belongs to oblique system under the room temperature, and spacer is P2
1/ c, unit cell parameters is a=17.508 (5)
B=7.607 (2)
C=13.533 (4)
α=γ=90.0 °, β=93.712 (6) °, Z=4, V=1798.4 (10)
Material undergoes phase transition in the time of 47 ℃, and the transformation temperature scope is 47～55 ℃, and the latent heat in the phase transition process is greater than 2000J/mol, and phase transition process is reversible; Spacer is P2 within being higher than 47 ℃ temperature range
1/ c, unit cell parameters is: a=7.190 (9)
B=7.698 (10)
C=34.08 (4)
β=90.05 (4) °, V=1886 (4)
This material structure formula is:
2. the preparation method of phase change material as claimed in claim 1, it is characterized in that: 4-(4-dimethylamino styryl) picoline iodide and three fluosulfonic acid silver carry out ion exchange reaction in the aqueous solution, through stirring, filtration, washing, natural air drying, obtain target product.
3. the phase change material of claim 1 is used for energy storage means and energy conserving system.
4. the purposes of phase change material claimed in claim 3 is characterized in that: this material is used for the preparation of controlled dielectric electric capacity, controlled dielectric grating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110325485.8A CN103059814B (en) | 2011-10-21 | A kind of phase-change material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110325485.8A CN103059814B (en) | 2011-10-21 | A kind of phase-change material |
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| Publication Number | Publication Date |
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| CN103059814A true CN103059814A (en) | 2013-04-24 |
| CN103059814B CN103059814B (en) | 2016-12-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342778A (en) * | 2018-01-30 | 2018-07-31 | 萍乡学院 | Double dichloroacetic acid potassium of phase twin crystal and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999025894A1 (en) * | 1997-11-17 | 1999-05-27 | The Trustees Of Princeton University | Low pressure vapor phase deposition of organic thin films |
| CN101823995A (en) * | 2010-03-31 | 2010-09-08 | 北京科技大学 | 4-(4-dimethylaminostyryl) picoline3-carboxyl-4-hydroxy benzene sulfonate, nonlinear optical crystal and preparation method thereof |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999025894A1 (en) * | 1997-11-17 | 1999-05-27 | The Trustees Of Princeton University | Low pressure vapor phase deposition of organic thin films |
| CN101823995A (en) * | 2010-03-31 | 2010-09-08 | 北京科技大学 | 4-(4-dimethylaminostyryl) picoline3-carboxyl-4-hydroxy benzene sulfonate, nonlinear optical crystal and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342778A (en) * | 2018-01-30 | 2018-07-31 | 萍乡学院 | Double dichloroacetic acid potassium of phase twin crystal and preparation method thereof |
| CN108342778B (en) * | 2018-01-30 | 2020-07-17 | 萍乡学院 | Phase-change crystal potassium bis (dichloroacetate) and preparation method thereof |
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