CN103183862A - High-thermal-conductivity phase-change composite material and preparation process thereof - Google Patents
High-thermal-conductivity phase-change composite material and preparation process thereof Download PDFInfo
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- CN103183862A CN103183862A CN2013100934948A CN201310093494A CN103183862A CN 103183862 A CN103183862 A CN 103183862A CN 2013100934948 A CN2013100934948 A CN 2013100934948A CN 201310093494 A CN201310093494 A CN 201310093494A CN 103183862 A CN103183862 A CN 103183862A
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Abstract
A high-thermal-conductivity phase-change composite material comprises the following raw materials according to mass ratio: 5-20% of expanded graphite, 30-40% of high-density polyethylene, and 40-65% of phase-change microcapsule. The high-thermal-conductivity phase-change composite material and a preparation process have the advantages that the thermal conductivity is high, and no liquid overflows in phase change.
Description
Technical field
The invention belongs to a kind of phase change composite material and preparation technology thereof, especially relate to a kind of high heat conduction phase change composite material and preparation technology thereof.
Background technology
Absorb or discharge a large amount of heats when phase-changing energy storage material undergoes phase transition by material, realize storage and the utilization of energy, can effectively solve supply and demand unmatched contradiction on time and space.Phase change energy storage technology is widely used in having discontinuity or instable heat management field, as the heat management of aerospace large power assembly, the field such as recycling, energy saving building of heat radiation, sun power utilization, industrial waste heat waste heat during the cyclical intermission formula work electronics.
Phase-change microcapsule is to use the New-type phase change matrix material with nucleocapsid structure that microcapsulary constitutes at the polymeric membrane of solid-liquid phase change particles of material surface coating one deck stable performance, its cyst material is insoluble not molten polymkeric substance, and the Nang core is that phase change material is crystalline hydrate salt, paraffin, straight-chain paraffin, polyoxyethylene glycol etc.The material that undergoes phase transition in phase-change microcapsule is closed in the ball-type capsule, thereby can effectively solve phase change material leakage, be separated and problem such as corrodibility, be conducive to improve the application performance of phase change material, and can widen phase-transition heat-storage The Application of Technology field.The application of phase-change microcapsule mainly can be divided into both direction: the one, and the latent heat when utilizing its phase transformation mixes it with heat-transfer fluid, improve the thermal capacitance of heat-transfer fluid, is used for heat transmission, refrigerant etc.; The 2nd, utilize its phase change temperature control characteristic, be applied to textiles, buildings, mark simulation and stealthy etc., improve thermal protection or regulate temperature.The research of the polymer-based carbon stable phase change composite material that is composited about phase-change microcapsule, heat conduction toughener and polymkeric substance is few.People such as Li Jianli are matrix with wood powder/high density polyethylene(HDPE) compound system, add phase-change microcapsule, heat conduction toughener, interface modifier and other auxiliary agent of different content, compression molding at other.Though added crystalline flake graphite heat conduction toughener, it is also little to the contribution that thermal conductivity improves.When the content of crystalline flake graphite was 8.8%, thermal conductivity had but only improved 17.7%.
Summary of the invention
At present the deficiencies in the prior art and defective, the purpose of this invention is to provide a kind of thermal conductivity height, high heat conduction phase change composite material of the setting that absence of liquid is overflowed during phase transformation and preparation method thereof.
Phase-change microcapsule has higher potential heat value, and high density polyethylene(HDPE) is a kind of good binding agent, with phase-change microcapsule, cohesiveness and consistency that expanded graphite is good, and the structure of phase-change microcapsule is not had destruction.Expanded graphite has high thermal and specific surface area, can be in wet ball grinding technology and high density polyethylene(HDPE), and phase-change microcapsule mixes very even.Phase-change microcapsule, high density polyethylene(HDPE) and expanded graphite place ball grinder according to certain mass ratio, adopt wet ball grinding technology to mix, and be hot-forming after the vacuum-drying.
Technical scheme of the present invention is as follows
The composition of raw materials mass ratio of the high heat conduction phase change composite material of the present invention is: expanded graphite is 5-20%, and high density polyethylene(HDPE) is 30%-40%, and phase-change microcapsule is 40-65%.
The expanded graphite that adopts with natural flake graphite as raw material, perchloric acid as intercalator, concentrated nitric acid as auxiliary agent, adopt acidifying, washing, separation, drying, processes such as expanded to form.Concrete preparation method see document (Wei Xinghai, Liu Lang, Zhang Jinxi, etc. the preparation of HClO4-GIC and the performance of soft graphite thereof. novel charcoal material. 2007,22,342-348.).
High density polyethylene(HDPE) adopts Beijing profit to be 1789 types that trade company produces of doing business, and is Powdered.
Aforesaid phase-change microcapsule is selected U.S. microtek laboratories for use, and MPCM 37 D that inc. produces are Powdered.
The preparation technology of high heat conduction phase change composite material proposed by the invention is:
(1) expanded graphite forms the expanded graphite powder shape after the high speed kneader is pulverized, and particle size range is the 50-500 micron;
(2) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden by composition of raw materials;
(3) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 150-300min, and the particle diameter of mixture is the 5-200 micron behind the ball milling;
(4) mixture behind the ball milling mixing carries out vacuum-drying, forms the dry mixed powder;
(5) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 100-150 ℃, and forming pressure is 10-30MPa, and the heat-insulation pressure keeping time is 100-150min, obtains high heat conduction phase change composite material.
The model of aforesaid high speed kneader is GH-10DY, manufacturer's Beijing Ying Te plastics machinery head factory.
The QM-BP planetary ball mill that aforesaid ball mill selects for use Nanjing Univ. Instrument Factory to produce, wet ball grinding technology is not destroyed the structure of phase-change microcapsule.
The present invention is melamine formaldehyde resin because of the cyst wall of the phase-change microcapsule that adopts, the mold temperature 100-150 ℃ of structure that can not destroy phase-change microcapsule.
A kind of high heat conduction phase change composite material of the present invention and preparation technology thereof, the normal temperature thermal conductivity of the matrix material that it is prepared is 0.9-10W/m K.This matrix material can be used as the cooling of electronic component.
The present invention compared with prior art has following advantage:
1. this invention is that phase change material is compared with the phase change composite material of no phase-change microcapsule with the phase-change microcapsule, and absence of liquid is overflowed advantage when having phase transformation;
2. this invention adopts wet ball grinding technology to compare with adopting high speed kneader hybrid technique, has the more even advantage of mixing;
3. this invention employing expanded graphite is compared as the heat conduction toughener with the employing crystalline flake graphite as the heat conduction toughener and is had the more obvious advantage of heat conduction reinforced effects;
4. this invention adopts hot press forming technology, but has the processed-type advantage.
Embodiment
Embodiment 1: concrete preparation process is as follows:
(1) expanded graphite with natural flake graphite as raw material, perchloric acid as intercalator, concentrated nitric acid as auxiliary agent, adopt acidifying, washing, separation, drying, processes such as expanded to form.Wherein the mass ratio of natural flake graphite, perchloric acid, concentrated nitric acid adding is 1:4:0.2.Acidifying is 10 hours under normal temperature, and with the pure water washing, centrifugation is 10 minutes then, and repeatedly washing and centrifugation is up to neutrality.Then 100 ℃ of following vacuum-dryings 1 hour.Sample after the vacuum-drying places 900 ℃ retort furnace interior expanded.
(2) form the expanded graphite powder shape after the high speed kneader is pulverized, particle size range is the 200-500 micron; The model of the high speed kneader that this process adopts is GH-10DY, manufacturer's Beijing Ying Te plastics machinery head factory;
(3) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden according to mass ratio 5:40:55; The high density polyethylene(HDPE) that adopts adopts Beijing profit to be 1789 types that trade company produces of doing business, and is Powdered.Phase-change microcapsule is selected U.S. microtek laboratories for use, and MPCM 37 D that inc. produces are Powdered;
(4) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 150min, and the particle diameter of mixture is the 50-150 micron behind the ball milling; The QM-BP planetary ball mill that the used ball mill of this process selects for use Nanjing Univ. Instrument Factory to produce;
(5) mixture behind the ball milling mixing carries out vacuum-drying, forms the dry mixed powder;
(6) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 110 ℃, and forming pressure is 20MPa, and the heat-insulation pressure keeping time is 100min, obtains high heat conduction phase change composite material.
Prepared composite property is as follows:
Density: 0.87g/cm
3Thermal conductivity: 0.94W/m K.
Embodiment 2: concrete preparation process is as follows:
(1), (2) and (5) are with embodiment 1;
(3) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden according to mass ratio 10:40:50; Selected sample is with embodiment 1;
(4) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 180min, and the particle diameter of mixture is the 50-200 micron behind the ball milling; Select for use ball mill with embodiment 1;
(6) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 100 ℃, and forming pressure is 15MPa, and the heat-insulation pressure keeping time is 130min, obtains high heat conduction phase change composite material.
Prepared composite property is as follows:
Density: 0.92g/cm
3Thermal conductivity: 4.59W/m K.
Embodiment 3: concrete preparation process is as follows:
(1), (2) and (5) are with embodiment 1;
(3) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden according to mass ratio 15:40:45; Selected sample is with embodiment 1;
(4) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 200min, and the particle diameter of mixture is the 80-220 micron behind the ball milling; Select for use ball mill with embodiment 1;
(6) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 120 ℃, and forming pressure is 25MPa, and the heat-insulation pressure keeping time is 140min, obtains high heat conduction phase change composite material.
Prepared composite property is as follows:
Density: 1.02g/cm
3Thermal conductivity: 6.01W/m K.
Embodiment 4:
(1), (2) and (5) are with embodiment 1;
(3) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden according to mass ratio 20:35:45; Selected sample is with embodiment 1;
(4) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 180min, and the particle diameter of mixture is the 90-250 micron behind the ball milling; Select for use ball mill with embodiment 1;
(6) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 110 ℃, and forming pressure is 30MPa, and the heat-insulation pressure keeping time is 120min, obtains high heat conduction phase change composite material.
Prepared composite property is as follows:
Density: 1.0g/cm
3Thermal conductivity: 9.9W/m K.
Claims (7)
1. one kind high heat conduction phase change composite material, it is characterized in that the composition of raw materials mass ratio of high heat conduction phase change composite material is: expanded graphite is 5-20%, and high density polyethylene(HDPE) is 30%-40%, and phase-change microcapsule is 40-65%.
2. a kind of high heat conduction phase change composite material as claimed in claim 1, it is characterized in that described expanded graphite with natural flake graphite as raw material, perchloric acid as intercalator, concentrated nitric acid as auxiliary agent, adopt acidifying, washing, separation, drying, processes such as expanded to form.
3. a kind of high heat conduction phase change composite material as claimed in claim 1 is characterized in that described high density polyethylene(HDPE) adopts Beijing profit to be 1789 types that trade company produces of doing business, and is Powdered.
4. a kind of high heat conduction phase change composite material as claimed in claim 1 is characterized in that described phase-change microcapsule selects U.S. microtek laboratories for use, and MPCM 37 D that inc. produces are Powdered.
5. as the preparation method of each described a kind of high heat conduction phase change composite material of claim 1-4, it is characterized in that comprising the steps:
(1) expanded graphite forms the expanded graphite powder shape after the high speed kneader is pulverized, and particle size range is the 50-500 micron;
(2) expanded graphite powder, Powdered high density polyethylene(HDPE), Powdered phase-change microcapsule carry out preparing burden by composition of raw materials;
(3) mixture for preparing is packed in the ball mill, add dehydrated alcohol, carry out wet ball grinding, the time is 150-300min, and the particle diameter of mixture is the 5-200 micron behind the ball milling;
(4) mixture behind the ball milling mixing carries out vacuum-drying, forms the dry mixed powder;
(5) mixed powder is packed in the compression molding mould, hot-forming, mold temperature is 100-150 ℃, and forming pressure is 10-30MPa, and the heat-insulation pressure keeping time is 100-150min, obtains high heat conduction phase change composite material.
6. the preparation method of a kind of high heat conduction phase change composite material as claimed in claim 5, the model that it is characterized in that described high speed kneader is GH-10DY, manufacturer's Beijing Ying Te plastics machinery head factory.
7. the preparation method of a kind of high heat conduction phase change composite material as claimed in claim 5 is characterized in that the QM-BP planetary ball mill that described ball mill selects for use Nanjing Univ. Instrument Factory to produce.
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Cited By (8)
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| CN103773322A (en) * | 2014-02-08 | 2014-05-07 | 中国电子科技集团公司第三十三研究所 | Phase change microcapsule heat conduction material and preparation method thereof |
| CN103849356A (en) * | 2014-03-20 | 2014-06-11 | 中国电子科技集团公司第三十三研究所 | Electrical insulating phase-change heat conducting material and preparation method thereof |
| CN104650812A (en) * | 2013-11-18 | 2015-05-27 | 北京科技大学 | Method for preparing stearic acid-silica composite phase-change heat storage slurry |
| CN105147445A (en) * | 2015-09-30 | 2015-12-16 | 河南省超亚医药器械有限公司 | Intelligent constant-temperature hot-compressing patch |
| CN105805819A (en) * | 2016-05-10 | 2016-07-27 | 厦门大学嘉庚学院 | Novel solar floor heating system based on phase change material |
| CN110408366A (en) * | 2019-07-12 | 2019-11-05 | 南方科技大学 | A kind of core-shell structure phase-change material and preparation method thereof |
| CN114456774A (en) * | 2022-01-11 | 2022-05-10 | 湖北工业大学 | Shell-encapsulated microcapsule phase change material and preparation method and application thereof |
| CN115093832A (en) * | 2022-06-09 | 2022-09-23 | 武汉中科先进材料科技有限公司 | Preparation method of environment-friendly heat-insulation temperature-control flame-retardant material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650812A (en) * | 2013-11-18 | 2015-05-27 | 北京科技大学 | Method for preparing stearic acid-silica composite phase-change heat storage slurry |
| CN104650812B (en) * | 2013-11-18 | 2018-04-03 | 北京科技大学 | A kind of method for preparing stearic acid silica composite phase-change heat-storage slurry |
| CN103773322A (en) * | 2014-02-08 | 2014-05-07 | 中国电子科技集团公司第三十三研究所 | Phase change microcapsule heat conduction material and preparation method thereof |
| CN103849356A (en) * | 2014-03-20 | 2014-06-11 | 中国电子科技集团公司第三十三研究所 | Electrical insulating phase-change heat conducting material and preparation method thereof |
| CN105147445A (en) * | 2015-09-30 | 2015-12-16 | 河南省超亚医药器械有限公司 | Intelligent constant-temperature hot-compressing patch |
| CN105147445B (en) * | 2015-09-30 | 2017-06-16 | 张亚超 | Intelligent constant-temperature hot compress paste |
| CN105805819A (en) * | 2016-05-10 | 2016-07-27 | 厦门大学嘉庚学院 | Novel solar floor heating system based on phase change material |
| CN110408366A (en) * | 2019-07-12 | 2019-11-05 | 南方科技大学 | A kind of core-shell structure phase-change material and preparation method thereof |
| CN114456774A (en) * | 2022-01-11 | 2022-05-10 | 湖北工业大学 | Shell-encapsulated microcapsule phase change material and preparation method and application thereof |
| CN115093832A (en) * | 2022-06-09 | 2022-09-23 | 武汉中科先进材料科技有限公司 | Preparation method of environment-friendly heat-insulation temperature-control flame-retardant material |
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Application publication date: 20130703 |