CN105349107A - Preparation method for expandable graphite/capric acid-lauric acid-oleic acid composite phase change material - Google Patents

Preparation method for expandable graphite/capric acid-lauric acid-oleic acid composite phase change material Download PDF

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Publication number
CN105349107A
CN105349107A CN201510670176.2A CN201510670176A CN105349107A CN 105349107 A CN105349107 A CN 105349107A CN 201510670176 A CN201510670176 A CN 201510670176A CN 105349107 A CN105349107 A CN 105349107A
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China
Prior art keywords
acid
change material
expanded graphite
composite phase
oleic acid
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CN201510670176.2A
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杨志
汤雪辉
张薇
朱备
翟晓强
张亚非
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063Materials absorbing or liberating heat during crystallisation; Heat storage materials

Abstract

The invention discloses a preparation method for an expandable graphite/capric acid-lauric acid-oleic acid composite phase change material. The method comprises the following steps: uniformly mixing capric acid, lauric acid and oleic acid according to a proper proportion at a proper mixing temperature so as to obtain mixed acid with a certain solid-liquid phase change temperature; then with expandable graphite as a matrix material, impregnating the expandable graphite in the mixed acid at a proper impregnation temperature; and finally, removing incompletely impregnated mixed acid so as to obtain the expandable graphite/capric acid-lauric acid-oleic acid composite phase change material. The method is simple and has good practicality; and the prepared composite phase change material is in a solid state, has great enthalpy and high thermal conductivity, is convenient for large-scale industrial production and shows great application potential in the fields of constructional materials, heating and ventilation air conditioners.

Description

A kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material
Technical field
The present invention relates to a kind of preparation method of composite phase-change material, be specifically related to a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
Background technology
Phase change material utilizes the phase in version process storage/release latent heat of material, can temperature be controlled in specific range of temperatures, be a kind of green material of energy-conserving and environment-protective, be widely used in the fields such as intelligent temperature-regulation garment, electron device, building energy conservation, waste heat recovery, lagging material, heating ventilation air-conditioning system just gradually.Traditional solid-liquid phase change material is divided into inorganic solid-liquid phase change material and organic solid-liquid phase change material, although inorganic solid-liquid phase change material energy storage density is large, cheap, and material was easily occurring phenomenon that is cold and that be separated after repeatedly phase transition process.Therefore, organic solid-liquid phase change material becomes the focus of research because of advantage that its stable performance, transformation temperature easily regulate.
In recent years, the organic solid-liquid phase change material of high temperature is paid close attention to widely, paraffin is as common are machine solid-liquid phase change material (SolarEnergyMaterialsandSolarCells2014,128,447-455), its transformation temperature is generally positioned at 50 DEG C, simultaneously, its thermal conductivity is only about 0.2W/mK, and there is very large defect in room temperature phase-change application aspect, the poor thermal conductivity of material also can hinder material to directly apply to the low-temperature phase-change material fields such as heating ventilation air-conditioning system.Meanwhile, low-temperature phase-change material at room temperature presents liquid state, and the seepage of liquid is also problem demanding prompt solution.
Summary of the invention
Technical problem to be solved by this invention is: overcome above-mentioned the deficiencies in the prior art, proposes a kind of novel method preparing composite phase-change material.Ensure that the transformation temperature of material is positioned at about 20 DEG C, improve the thermal conductivity of material, prevent the seepage of phase change material simultaneously.
For achieving the above object, the invention provides a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material, capric acid, lauric acid and oleic acid is utilized to be uniformly mixed to form congruent melting nitration mixture, its transformation temperature is made to be positioned at about 20 DEG C, utilize expanded graphite as thermally conductive material afterwards, improve the thermal conductivity of nitration mixture, simultaneously because expanded graphite has the pore passage structure of good micron level, liquid nitration mixture by wicking action fully load between the duct of expanded graphite, thus reach good antiseep effect.Concrete technical scheme is as follows:
Prepare a method for expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material, comprise the following steps:
Step 1, by capric acid, lauric acid and oleic acid with proper ratio Homogeneous phase mixing under suitable mixing temperature, obtains the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, take expanded graphite as body material, under suitable dipping temperature, floods nitration mixture;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
Preferably, in step 1, capric acid and lauric mass ratio are 50:50 or 60:40 or 70:30 or 80:20 or 90:10.Oleic acid consumption is 0.01 ~ 0.2 times of capric acid and lauric acid total mass.
Preferably, adopting water-bath or oil bath to control mixing temperature in step 1 is 30 ~ 80 DEG C.The time of capric acid, lauric acid and oleic acid mixing is 5 ~ 30min.
Preferably, in step 2, expanded graphite order number is 30 ~ 150 orders.The mass ratio of expanded graphite and nitration mixture is 1:5 ~ 1:50.
Preferably, adopting water-bath or oil bath to control dipping temperature in step 2 is 30 ~ 80 DEG C.The time that expanded graphite floods in nitration mixture is 20 ~ 50min.
Compared with prior art, the present invention has following beneficial effect: technique is simple, practical, is convenient to large-scale commercial production.Meanwhile, the expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material transformation temperature of gained is positioned at about 20 DEG C (18 ~ 21 DEG C), and thermal conductivity is high, ne-leakage phenomenon in storage/heat release working cycle.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the present invention prepares expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material;
Fig. 2 is the SEM test pattern of expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material (expanded graphite and nitration mixture mass ratio are 1:5) prepared by a preferred embodiment of the present invention;
Fig. 3 is the SEM test pattern of expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material (expanded graphite and nitration mixture mass ratio are 1:35) prepared by another preferred embodiment of the present invention.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, mixes capric acid, lauric acid and oleic acid with the mass ratio of 60:40:5, and 30 DEG C of water-bath 30min, obtain the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, with 30 object expanded graphites for body material, gets expanded graphite and nitration mixture mass ratio is 1:5, mixes 40min, be fully impregnated into expanded graphite to make nitration mixture under 50 DEG C of water-baths;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
Embodiment 2
Step 1, mixes capric acid, lauric acid and oleic acid with the mass ratio of 70:30:8, and 50 DEG C of water-bath 10min, obtain the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, with 30 object expanded graphites for body material, gets expanded graphite and nitration mixture mass ratio is 1:5, mixes 30min, be fully impregnated into expanded graphite to make nitration mixture under 75 DEG C of water-baths;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
Embodiment 3
Step 1, mixes capric acid, lauric acid and oleic acid with the mass ratio of 90:10:12, and 50 DEG C of water-bath 15min, obtain the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, with 80 object expanded graphites for body material, gets expanded graphite and nitration mixture mass ratio is 1:35, mixes 50min, be fully impregnated into expanded graphite to make nitration mixture under 40 DEG C of water-baths;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
Embodiment 4
Step 1, mixes capric acid, lauric acid and oleic acid with the mass ratio of 80:20:15, and 30 DEG C of water-bath 50min, obtain the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, with 120 object expanded graphites for body material, gets expanded graphite and nitration mixture mass ratio is 1:35, mixes 20min, be fully impregnated into expanded graphite to make nitration mixture under 80 DEG C of water-baths;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.

Claims (10)

1. prepare a method for expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material, it is characterized in that, comprise the following steps:
Step 1, by capric acid, lauric acid and oleic acid with proper ratio Homogeneous phase mixing under suitable mixing temperature, obtains the nitration mixture that solid-liquid phase change temperature is certain;
Step 2, take expanded graphite as body material, under suitable dipping temperature, floods described nitration mixture;
Step 3, removes the nitration mixture of non-thorough impregnation, obtains described expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material.
2. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, it is characterized in that, capric acid described in step 1 and described lauric mass ratio are 50:50 or 60:40 or 70:30 or 80:20 or 90:10.
3. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, is characterized in that, described oleic acid consumption is 0.01 ~ 0.2 times of described capric acid and described lauric acid total mass.
4. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, is characterized in that, the time of capric acid described in step 1, described lauric acid and described oleic acid mixing is 5 ~ 30min.
5. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, is characterized in that, adopting water-bath or oil bath to control described mixing temperature in step 1 is 30 ~ 80 DEG C.
6. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, it is characterized in that, the order of expanded graphite described in step 2 number is 30 ~ 150 orders.
7. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, it is characterized in that, the mass ratio of expanded graphite described in step 2 and described nitration mixture is 1:5 ~ 1:50.
8. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, is characterized in that, adopting water-bath or oil bath to control described dipping temperature in step 2 is 30 ~ 80 DEG C.
9. a kind of method preparing expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material according to claim 1, it is characterized in that, the time of the described dipping in step 2 is 20 ~ 50min.
10. expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material that the preparation method according to any one of claim 1 ~ 9 prepares, is characterized in that, the transformation temperature of described expanded graphite/capric acid-lauric acid-oleic acid composite phase-change material is 18 ~ 21 DEG C.
CN201510670176.2A 2015-10-13 2015-10-13 Preparation method for expandable graphite/capric acid-lauric acid-oleic acid composite phase change material Pending CN105349107A (en)

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CN106398651A (en) * 2016-09-09 2017-02-15 成都九十度工业产品设计有限公司 Solid-liquid phase change material for automotive heat insulation mat
CN113372809A (en) * 2021-04-23 2021-09-10 浙江工商大学 Intelligent heat-insulating coating and preparation and application thereof
CN115404046A (en) * 2022-08-30 2022-11-29 西安交通大学 Flexible composite phase change material suitable for battery thermal management and preparation method and application thereof

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106398651A (en) * 2016-09-09 2017-02-15 成都九十度工业产品设计有限公司 Solid-liquid phase change material for automotive heat insulation mat
CN106398651B (en) * 2016-09-09 2019-04-16 成都九十度工业产品设计有限公司 A kind of solid-liquid phase change material for car heat insulating pad
CN113372809A (en) * 2021-04-23 2021-09-10 浙江工商大学 Intelligent heat-insulating coating and preparation and application thereof
CN115404046A (en) * 2022-08-30 2022-11-29 西安交通大学 Flexible composite phase change material suitable for battery thermal management and preparation method and application thereof

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