CN111826127A - Preparation method of paraffin graphite flake and expanded graphite composite phase change material - Google Patents

Preparation method of paraffin graphite flake and expanded graphite composite phase change material Download PDF

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Publication number
CN111826127A
CN111826127A CN202010573908.7A CN202010573908A CN111826127A CN 111826127 A CN111826127 A CN 111826127A CN 202010573908 A CN202010573908 A CN 202010573908A CN 111826127 A CN111826127 A CN 111826127A
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China
Prior art keywords
paraffin
expanded graphite
graphite
change material
phase change
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CN202010573908.7A
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Chinese (zh)
Inventor
李强
胡定华
许肖永
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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Priority to CN202010573908.7A priority Critical patent/CN111826127A/en
Publication of CN111826127A publication Critical patent/CN111826127A/en
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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
    • 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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular

Abstract

The invention provides a preparation method of a paraffin graphite flake and expanded graphite composite phase-change material, which comprises the following steps of mixing expanded graphite with paraffin; then stirring and mixing the cut graphite sheets with the paraffin expanded graphite under the heating condition; and finally, compressing and molding the paraffin graphite flake and expanded graphite composite phase change material in a mold to obtain the paraffin graphite flake and expanded graphite composite phase change material. The mass of the expanded graphite accounts for 10-20%, the mass of the paraffin accounts for 80-90%, and the thermal conductivity of the paraffin expanded graphite composite phase-change material can be improved.

Description

Preparation method of paraffin graphite flake and expanded graphite composite phase change material
Technical Field
The invention belongs to the field of preparation of paraffin composite phase change materials, and particularly relates to a preparation method of a paraffin expanded graphite sheet composite phase change material.
Background
The paraffin serves as a latent heat type heat energy storage material and plays an important role in improving the utilization efficiency of heat energy and developing renewable energy sources. Because the phase-change material has the advantages of large heat storage density, relatively constant working temperature and the like, the contradiction that the energy utilization is not matched in time and space can be effectively relieved. The paraffin phase-change material is widely used as an energy storage material due to the advantages of low cost, stability, high energy storage density, no toxicity and no corrosiveness. However, the paraffin phase-change material also has some disadvantages, such as large solid-liquid volume difference in the phase-change process, easy occurrence of liquid phase leakage, and relatively low heat conductivity coefficient, which limits the large-scale application of the paraffin phase-change material, so that the development of the high heat conductivity phase-change material has great value. The expanded graphite is used as the best matrix material due to excellent wettability with organic phase change materials, large specific surface area and good heat conductivity. Therefore, extensive studies have been made on the composite phase change materials based on expanded graphite.
The preparation method of the paraffin composite phase-change material for enhancing the heat conductivity usually comprises the steps of adding heat-conducting nano particles or combining paraffin and foam-bath metal. And adding heat-conducting nano particles, namely melting the paraffin and uniformly mixing the melted paraffin with the heat-conducting nano material by stirring or ultrasonic waves. Mixing the paraffin and the foam-bath metal, namely heating and melting the paraffin, and then combining the paraffin and the foam-bath metal by adopting a vacuum infiltration method. The two methods can increase the heat conductivity of the composite phase-change material, and have the following common defects: in the phase change process, the material leaks and loses the composite effect, and meanwhile, the addition of other materials can reduce the phase change latent heat of the material and influence the use effect.
Disclosure of Invention
The invention aims to provide a preparation method of a paraffin expanded graphite and graphite sheet composite phase-change material, which aims to improve the thermal conductivity of the paraffin expanded graphite and graphite sheet composite phase-change material.
The technical solution for realizing the purpose of the invention is as follows:
a preparation method of a paraffin graphite sheet and expanded graphite composite phase-change material comprises the following steps:
s1, mixing the expanded graphite with paraffin;
s2, heating, stirring and mixing the cut graphite sheets and the paraffin expanded graphite;
s3, compressing and molding the paraffin graphite sheet and expanded graphite composite phase change material in a mold to obtain the paraffin graphite sheet and expanded graphite composite phase change material.
Compared with the prior art, the invention has the following remarkable advantages:
(1) by adding the expanded graphite, the heat-conducting property of the phase-change material can be effectively improved, and meanwhile, the phase-change material is prevented from being leaked.
(2) Through adding the graphite flake, when effectively improving heat conduction, can realize the better heat conductivility under the condition of same phase transition latent heat.
Drawings
Fig. 1 is a flow chart of a preparation method of the paraffin graphite sheet expanded graphite composite phase change material provided by the invention.
Fig. 2 is an in-plane thermal conductivity test chart of the composite phase change material with different addition amounts of the expanded graphite provided by the invention.
FIG. 3 is a phase change latent heat test chart of composite phase change materials with different addition amounts of expanded graphite.
Fig. 4 is a thermal conductivity test chart of the composite phase change material with different graphite sheet addition amounts provided by the invention.
FIG. 5 is a phase change latent heat test chart of composite phase change materials with different graphite sheet addition amounts.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
With reference to fig. 1, the preparation method of the paraffin expanded graphite sheet composite phase change material of the invention comprises the following steps:
s1, mixing the expanded graphite with paraffin;
in the present invention, the expanded graphite is prepared by a high-temperature expansion method or a microwave expansion method and using expandable graphite. The high-temperature expansion method generally adopts a high-temperature furnace for heating, and the expansion graphite is obtained under the condition of 900 ℃ for 30 s.
Specifically, firstly, paraffin blocks are mixed with the prepared expanded graphite, wherein the mass ratio of the expanded graphite is 10-20%, and the mass ratio of the paraffin is 90-80%, then the material is placed into a vacuum box for vacuumizing, heated to 70-80 ℃, and vacuum infiltration is carried out for 2-5 hours, so that the paraffin is completely absorbed by the expanded graphite.
S2, heating, stirring and mixing the cut graphite sheets and the paraffin expanded graphite;
specifically, the expanded graphite paraffin composite material prepared in S1 was mixed with a graphite sheet under stirring, the material was first heated to 80 ℃ and stirred for 15 minutes at a stirring rate of 100 rpm.
Specifically, the graphite sheet has a size of 30 mm × 2 mm and a thickness of 0.05 mm, wherein the mass ratio M of the graphite sheet to the expanded graphite is 0< M.ltoreq.0.5.
S3, compressing and molding the paraffin graphite sheet and expanded graphite composite phase change material in a mold to obtain the paraffin graphite sheet and expanded graphite composite phase change material.
Specifically, the pressure was 20MPa, and the pressing time was 5 minutes.
The invention is further illustrated by the following specific examples.
Example 1: a paraffin expanded graphite composite phase-change material comprises the following components in parts by mass: 8 percent of expanded graphite and 92 percent of paraffin; the preparation method comprises the following steps: firstly, cutting paraffin into blocks, uniformly stirring the blocks and the expanded graphite, adding the materials into a vacuum furnace, vacuumizing, heating to 80 ℃, heating for 2 hours, cooling, adding the paraffin expanded graphite composite material into a mold, and carrying out pressure forming under the pressure of 20Mpa for 5 minutes to finally obtain the paraffin expanded graphite composite phase-change material.
Example 2: the preparation method of the paraffin wax expanded graphite in this embodiment is basically the same as that in embodiment 1, except that the mass of the expanded graphite used in this embodiment is 10% and the mass of the paraffin wax is 90%.
Example 3: the preparation method of the paraffin wax expanded graphite in this embodiment is basically the same as that in embodiment 1, except that the mass of the expanded graphite used in this embodiment is 12% and the mass of the paraffin wax is 88%.
Example 4: the preparation method of the paraffin wax expanded graphite in this embodiment is basically the same as that in embodiment 1, except that the mass of the expanded graphite used in this embodiment is 14% and the mass of the paraffin wax is 86%.
Example 5: the method for producing paraffin-expanded graphite in this example was substantially the same as that in example 1, except that the expanded graphite used in this example was 16% by mass and the paraffin was 84% by mass.
Example 6: the method for producing paraffin wax-expanded graphite in this example was substantially the same as that in example 1, except that the expanded graphite used in this example was 18% by mass and the paraffin wax was 86% by mass.
Example 7: the method for producing paraffin-expanded graphite in this example was substantially the same as that in example 1, except that the expanded graphite used in this example was 20% by mass and the paraffin was 80% by mass.
Referring to fig. 2 and 3, it can be seen from the graphs that the heat conduction of the phase change material is obviously improved with the addition of the expanded graphite, but the latent heat of phase change is also reduced, so when the paraffin graphite flake expanded graphite composite phase change material is prepared, the mass ratio of the expanded graphite is recommended to be 10% -20%, and the mass ratio of the paraffin is recommended to be 90% -80%.
Example 8: a paraffin graphite sheet and expanded graphite composite phase-change material comprises the following components in parts by mass: 16% of expanded graphite and 84% of paraffin; the preparation method comprises the following steps: firstly, cutting paraffin into blocks and uniformly stirring the blocks and expanded graphite, adding the materials into a vacuum drying oven, vacuumizing and heating to 80 ℃, heating for 2 hours, and heating, stirring and mixing the cut graphite sheets and the paraffin expanded graphite, wherein the mass ratio of the graphite sheets to the expanded graphite is 1: and 4, cooling, adding the paraffin graphite sheet expanded graphite composite material into a mold, and carrying out pressure forming under the pressure of 20Mpa for 5 minutes to finally obtain the paraffin graphite sheet expanded graphite composite phase change material.
Example 9: the preparation method of the paraffin graphite sheet expanded graphite in the present embodiment is basically the same as the preparation method in embodiment 8, except that the mass ratio of the expanded sheets to the expanded graphite in the present embodiment is 3: 8.
example 10: the preparation method of the paraffin graphite sheet expanded graphite in the present embodiment is basically the same as the preparation method in embodiment 8, except that the mass ratio of the expanded sheets to the expanded graphite in the present embodiment is 1: 2.
with reference to fig. 4 and 5, it can be seen that the addition of graphite flakes can effectively improve the heat conductivity of the phase change material on the basis of the mass fraction of the expanded graphite being 16%, but the addition of graphite flakes can reduce the latent heat of phase change, so that when the paraffin graphite flake and expanded graphite composite phase change material is prepared, the mass ratio M of the graphite flakes to the expanded graphite is recommended, wherein M is more than 0 and less than or equal to 0.5.

Claims (6)

1. The preparation method of the paraffin graphite sheet and expanded graphite composite phase change material is characterized by comprising the following steps:
s1, mixing the expanded graphite with paraffin;
s2, stirring and mixing the cut graphite sheets with the paraffin expanded graphite under the heating condition;
s3, compressing and molding the paraffin graphite sheet and expanded graphite composite phase change material in a mold to obtain the paraffin graphite sheet and expanded graphite composite phase change material.
2. The method for preparing the phase change material of the paraffin graphite sheet and the expanded graphite as claimed in claim 1, wherein the mixing ratio of the graphite sheet to the paraffin expanded graphite in the step S1 is as follows: the mass ratio of the expanded graphite is 10-20 percent, and the mass ratio of the paraffin is 80-90 percent.
3. The method for preparing the phase change material of paraffine graphite sheet and expanded graphite composite according to claim 1, wherein the paraffin and the expanded graphite are mixed by a vacuum infiltration method in step S1.
4. The preparation method of the paraffingraphite sheet expanded graphite composite phase-change material according to claim 3, wherein the heating temperature for vacuum infiltration is 70-80 ℃, and the heating time is 2-5 hours.
5. The method for preparing the phase change material of the paraffingraphite sheet and the expanded graphite composite according to the claim 1, wherein the mass ratio M of the graphite sheet to the expanded graphite in the step S2 is 0< M < 0.5.
6. The method for preparing a phase change material of paraffine graphite sheet and expanded graphite composite according to claim 1, wherein the compression molding pressure of step S3 is 20MPa, and the pressing time is 5 minutes.
CN202010573908.7A 2020-06-22 2020-06-22 Preparation method of paraffin graphite flake and expanded graphite composite phase change material Pending CN111826127A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877036A (en) * 2021-01-26 2021-06-01 深圳市大通创新科技有限公司 Phase change material and preparation method and application thereof
CN114381237A (en) * 2022-01-07 2022-04-22 瑞声科技(南京)有限公司 Heat storage composite material and preparation method thereof
CN114656936A (en) * 2022-04-14 2022-06-24 南京航空航天大学 Preparation method of low-temperature environment heat-insulating material based on phase change regulation and control technology
CN114656939A (en) * 2022-05-10 2022-06-24 华南理工大学 Expanded graphite-based composite phase-change material with anisotropic thermal conductivity and preparation method thereof
CN115029109A (en) * 2022-06-24 2022-09-09 华南理工大学 High-fluidity high-thermal-conductivity composite phase change material, preparation method thereof and method for filling heat exchanger

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103059817A (en) * 2012-12-27 2013-04-24 东南大学 Composite shape-stabilized phase change material, preparation method and heat storage mortar prepared by using phase change material
CN106905928A (en) * 2017-03-24 2017-06-30 杭州龙灿液态金属科技有限公司 Packaged type phase-change energy-storage composite material and its processing technology with superelevation thermal conductivity
CN108300427A (en) * 2018-03-19 2018-07-20 唐山易达墨烯科技有限公司 Paraffin expanded graphite composite phase-changing material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103059817A (en) * 2012-12-27 2013-04-24 东南大学 Composite shape-stabilized phase change material, preparation method and heat storage mortar prepared by using phase change material
CN106905928A (en) * 2017-03-24 2017-06-30 杭州龙灿液态金属科技有限公司 Packaged type phase-change energy-storage composite material and its processing technology with superelevation thermal conductivity
CN108300427A (en) * 2018-03-19 2018-07-20 唐山易达墨烯科技有限公司 Paraffin expanded graphite composite phase-changing material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877036A (en) * 2021-01-26 2021-06-01 深圳市大通创新科技有限公司 Phase change material and preparation method and application thereof
CN114381237A (en) * 2022-01-07 2022-04-22 瑞声科技(南京)有限公司 Heat storage composite material and preparation method thereof
CN114656936A (en) * 2022-04-14 2022-06-24 南京航空航天大学 Preparation method of low-temperature environment heat-insulating material based on phase change regulation and control technology
CN114656939A (en) * 2022-05-10 2022-06-24 华南理工大学 Expanded graphite-based composite phase-change material with anisotropic thermal conductivity and preparation method thereof
CN115029109A (en) * 2022-06-24 2022-09-09 华南理工大学 High-fluidity high-thermal-conductivity composite phase change material, preparation method thereof and method for filling heat exchanger

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Application publication date: 20201027