技术领域technical field
本发明属于一种相变复合材料及其制备工艺，尤其是涉及一种高导热相变复合材料及其制备工艺。 The invention belongs to a phase-change composite material and a preparation process thereof, in particular to a phase-change composite material with high thermal conductivity and a preparation process thereof. the
背景技术Background technique
相变储能材料通过材料发生相变时吸收或释放大量热量，实现能量的存储和利用，可有效解决供求在时间和空间上不匹配的矛盾。相变储能技术被广泛应用于具有间断性或不稳定性的热管理领域，如航空航天大功率组件的热管理、周期性间歇式工作电子期间的散热、太阳能利用、工业废热余热的回收利用、节能建筑等领域。 Phase change energy storage materials absorb or release a large amount of heat when the material undergoes a phase change to realize energy storage and utilization, which can effectively solve the contradiction between supply and demand in terms of time and space. Phase change energy storage technology is widely used in intermittent or unstable thermal management fields, such as thermal management of aerospace high-power components, heat dissipation during periodic intermittent work electronics, solar energy utilization, and recycling of industrial waste heat and waste heat , energy-saving buildings and other fields. the
相变微胶囊是应用微胶囊技术在固-液相变材料微粒表面包覆一层性能稳定的高分子膜而构成的具有核壳结构的新型相变复合材料，它的囊壁材料为不溶不熔的聚合物，嚢芯即相变物质为结晶水合盐、石蜡、直链烷烃、聚乙二醇等。在相变微胶囊中发生相变的物质被封闭在球形胶囊中，从而可有效解决相变材料的泄漏、相分离以及腐蚀性等问题，有利于改善相变材料的应用性能，并可拓宽相变蓄热技术的应用领域。相变微胶囊的应用主要可以分为两个方向：一是利用其相变时的潜热，把它与传热流体混合，提高传热流体的热容，用于热量传输、冷却剂等；二是利用其相变温控特性，将其应用于纺织品、建筑物、标伪装隐身等，提高热防护性或者调节温度。关于相变微胶囊、导热增强剂与聚合物复合而成的聚合物基定形相变复合材料的研究不多。李建立等人以木粉/高密度聚乙烯复合体系为基体，在其他添加不同含量的相变微胶囊、导热增强剂、界面改性剂及其它助剂，模压成型。虽然加入了鳞片石墨导热增强剂，但是它对热导率提高的贡献并不大。当鳞片石墨的含量为8.8%时，热导率却仅仅提高了17.7%。 Phase change microcapsule is a new type of phase change composite material with a core-shell structure formed by coating a layer of stable polymer film on the surface of solid-liquid phase change material particles using microcapsule technology. Its capsule wall material is insoluble and insoluble The molten polymer, the capsule core or the phase change substance is crystalline hydrated salt, paraffin, straight-chain alkanes, polyethylene glycol, etc. The substance undergoing phase change in the phase change microcapsule is enclosed in a spherical capsule, which can effectively solve the problems of leakage, phase separation and corrosion of the phase change material, which is conducive to improving the application performance of the phase change material and broadening the range of phase change. Application field of heat storage technology. The application of phase change microcapsules can be mainly divided into two directions: one is to use the latent heat of phase change, mix it with heat transfer fluid, improve the heat capacity of heat transfer fluid, and use it for heat transfer, coolant, etc.; It is to use its phase change temperature control characteristics to apply it to textiles, buildings, camouflage and stealth, etc., to improve thermal protection or adjust temperature. There are not many studies on polymer-based shape-fixed phase-change composites composed of phase-change microcapsules, thermal conductivity enhancers and polymers. Li Jianli and others took the wood flour/high-density polyethylene composite system as the matrix, added different contents of phase change microcapsules, thermal conductivity enhancers, interface modifiers and other additives, and molded them. Although flake graphite thermal conductivity enhancer is added, it does not contribute much to the improvement of thermal conductivity. When the flake graphite content is 8.8%, the thermal conductivity is only increased by 17.7%. the
发明内容Contents of the invention
针对目前现有技术的不足和缺陷，本发明的目的是提供一种导热率高，相变时无液体溢出的定形高导热相变复合材料及其制备方法。 Aiming at the deficiencies and defects of the current prior art, the purpose of the present invention is to provide a high thermal conductivity phase change composite material with high thermal conductivity and no liquid overflow during phase change and its preparation method. the
相变微胶囊具有较高的潜热值,高密度聚乙烯是一种良好的粘结剂，与相变微胶囊、膨胀石墨良好的粘结性和相容性，而且对相变微胶囊的结构无破坏作用。膨胀石墨具有较高的热导率和比表面积，能在湿法球磨工艺中与高密度聚乙烯，相变微胶囊混合很均匀。相变微胶囊、高密度聚乙烯与膨胀石墨按照一定的质量比置于球磨罐中，采用湿法球磨工艺混合均匀，真空干燥后热压成型。 Phase-change microcapsules have a high latent heat value, and high-density polyethylene is a good binder, which has good adhesion and compatibility with phase-change microcapsules and expanded graphite. No destructive effect. Expanded graphite has high thermal conductivity and specific surface area, and can be mixed evenly with high-density polyethylene and phase change microcapsules in the wet ball milling process. Phase-change microcapsules, high-density polyethylene and expanded graphite are placed in a ball mill tank according to a certain mass ratio, mixed evenly by wet ball milling process, vacuum dried, and then hot-pressed. the
本发明的技术方案如下 The technical scheme of the present invention is as follows
本发明高导热相变复合材料的原料配方质量比为：膨胀石墨为5-20%，高密度聚乙烯为30%-40%，相变微胶囊为40-65%。The mass ratio of the raw material formula of the high thermal conductivity phase-change composite material of the invention is: 5-20% of expanded graphite, 30-40% of high-density polyethylene, and 40-65% of phase-change microcapsules.
所采用的膨胀石墨以天然鳞片石墨作为原料、高氯酸作为插层剂、浓硝酸作为助剂，采用酸化、水洗、分离、干燥、膨化等工艺加工而成。具体的制备方法见文献(魏兴海, 刘朗, 张金喜, 等. HClO4-GIC的制备及其柔性石墨的性能. 新型炭材料. 2007, 22, 342-348.)。 The expanded graphite used is made of natural flake graphite as raw material, perchloric acid as intercalation agent, concentrated nitric acid as auxiliary agent, and processed by acidification, washing, separation, drying, and expansion. The specific preparation method can be found in the literature (Wei Xinghai, Liu Lang, Zhang Jinxi, et al. Preparation of HClO4-GIC and its properties of flexible graphite. New carbon materials. 2007, 22, 342-348.). the
高密度聚乙烯采用北京利是行商贸公司生产的1789型，粉末状。 The high-density polyethylene adopts the 1789 type produced by Beijing Lishihang Trading Co., Ltd., in powder form. the
如上所述的相变微胶囊选用美国microtek laboratories, inc.生产的MPCM 37 D,粉末状。 The above-mentioned phase-change microcapsules select MPCM 37 D produced by U.S. microtek laboratories, inc., in powder form. the
本发明所提出的高导热相变复合材料的制备工艺为： The preparation process of the high thermal conductivity phase change composite material proposed by the present invention is:
(1)膨胀石墨经高速捏合机粉碎后形成膨胀石墨粉末状，粒径范围为50-500微米； (1) Expanded graphite is pulverized by a high-speed kneader to form expanded graphite powder, with a particle size range of 50-500 microns;
(2)膨胀石墨粉末、粉末状高密度聚乙烯、粉末状相变微胶囊进行按原料配方配料；(2) Expanded graphite powder, powdery high-density polyethylene, and powdery phase-change microcapsules are prepared according to the raw material formula;
(3)将配好的混合物装入球磨机中，加入无水乙醇，进行湿法球磨，时间为150-300min，球磨后混合物的粒径为5-200微米；(3) Put the prepared mixture into a ball mill, add absolute ethanol, and carry out wet ball milling for 150-300 minutes, and the particle size of the mixture after ball milling is 5-200 microns;
(4)球磨混匀后的混合物进行真空干燥，形成干燥混合粉体；(4) The mixture after ball milling and mixing is vacuum-dried to form a dry mixed powder;
(5)将混合粉体装入模压成型模具中，热压成型，成型温度为100-150℃，成型压力为10-30MPa，保温保压时间为100-150min，得到高导热相变复合材料。(5) Put the mixed powder into a compression molding mold, hot press molding, the molding temperature is 100-150°C, the molding pressure is 10-30MPa, the heat preservation and pressure holding time is 100-150min, and a high thermal conductivity phase change composite material is obtained.
如上所述的高速捏合机的型号为GH-10DY，生产厂家北京英特塑料机械总厂。 The model of the above-mentioned high-speed kneader is GH-10DY, and the manufacturer is Beijing Yingte Plastic Machinery General Factory. the
如上所述的球磨机选用南京大学仪器厂生产的QM-BP行星球磨机，湿法球磨工艺没有破坏相变微胶囊的结构。 The ball mill mentioned above is the QM-BP planetary ball mill produced by Nanjing University Instrument Factory, and the wet ball milling process does not destroy the structure of the phase change microcapsules. the
本发明因为所采用的相变微胶囊的囊壁为三聚氰胺-甲醛树脂，成型温度100-150℃不会破坏相变微胶囊的结构。Because the capsule wall of the phase-change microcapsule adopted in the present invention is melamine-formaldehyde resin, the molding temperature of 100-150 DEG C will not damage the structure of the phase-change microcapsule.
本发明所述一种高导热相变复合材料及其制备工艺，其所制备的复合材料的常温热导率为0.9-10W/m K。该复合材料可用作电子元件的冷却。 According to the high thermal conductivity phase change composite material and its preparation process of the present invention, the thermal conductivity of the composite material prepared by it is 0.9-10W/m K at room temperature. The composite material can be used as cooling for electronic components. the
本发明与现有技术相比具有如下优点： Compared with the prior art, the present invention has the following advantages:
1．本项发明以相变微胶囊为相变物质与无相变微胶囊的相变复合材料相比，具有相变时无液体溢出优点；1. Compared with the phase-change composite material without phase-change microcapsules, this invention has the advantage of no liquid overflowing during phase-change by using phase-change microcapsules as the phase-change material;
2．本项发明采用湿法球磨工艺与采用高速捏合机混合工艺相比，具有混合更均匀优点；2. Compared with the high-speed kneader mixing process, the invention adopts the wet ball milling process, which has the advantage of more uniform mixing;
3．本项发明采用膨胀石墨作为导热增强剂与采用鳞片石墨作为导热增强剂相比较具有导热增强效果更明显优点；3. Compared with the use of flake graphite as a thermal conductivity enhancer, the present invention has a more obvious advantage of thermal conductivity enhancement effect by using expanded graphite as a thermal conductivity enhancer;
4．本项发明采用热压成型工艺，具有可加工型优点。4. The invention adopts a hot pressing forming process and has the advantage of being machinable.
具体实施方式Detailed ways
实施例1：具体制备过程如下： Embodiment 1: The specific preparation process is as follows:
(1) 膨胀石墨以天然鳞片石墨作为原料、高氯酸作为插层剂、浓硝酸作为助剂，采用酸化、水洗、分离、干燥、膨化等工艺加工而成。其中天然鳞片石墨、高氯酸、浓硝酸加入的质量比为1：4：0.2。于常温下酸化10小时，用纯净水水洗，然后离心分离10分钟，多次水洗和离心分离，直到中性。然后在100℃下真空干燥1小时。真空干燥后的样品置于900℃的马弗炉内膨化。(1) Expanded graphite is made of natural flake graphite as raw material, perchloric acid as intercalation agent, concentrated nitric acid as auxiliary agent, and processed by acidification, washing, separation, drying, and expansion. Among them, the mass ratio of natural flake graphite, perchloric acid and concentrated nitric acid is 1:4:0.2. Acidify at room temperature for 10 hours, wash with pure water, and then centrifuge for 10 minutes, wash and centrifuge several times until neutral. It was then vacuum dried at 100° C. for 1 hour. The vacuum-dried samples were puffed in a muffle furnace at 900 °C.
(2)经高速捏合机粉碎后形成膨胀石墨粉末状，粒径范围为200-500微米；此过程所采用的高速捏合机的型号为GH-10DY，生产厂家北京英特塑料机械总厂； (2) form expanded graphite powder after being pulverized by a high-speed kneader, and the particle size range is 200-500 microns; the model of the high-speed kneader used in this process is GH-10DY, and the manufacturer is Beijing Inte Plastic Machinery General Factory;
(3)膨胀石墨粉末、粉末状高密度聚乙烯、粉末状相变微胶囊进行按照质量比5:40:55进行配料；所采用的高密度聚乙烯采用北京利是行商贸公司生产的1789型，粉末状。相变微胶囊选用美国microtek laboratories, inc.生产的MPCM 37 D,粉末状；(3) Expanded graphite powder, powdery high-density polyethylene, and powdery phase-change microcapsules are batched according to a mass ratio of 5:40:55; the high-density polyethylene used is the 1789 type produced by Beijing Lishihang Trading Company , powder form. The phase-change microcapsules are MPCM 37 D produced by Microtek Laboratories, Inc. in the United States, in powder form;
(4)将配好的混合物装入球磨机中，加入无水乙醇，进行湿法球磨，时间为150min，球磨后混合物的粒径为50-150微米；此过程所用的球磨机选用南京大学仪器厂生产的QM-BP行星球磨机；(4) Put the prepared mixture into a ball mill, add absolute ethanol, and carry out wet ball milling for 150 minutes. The particle size of the mixture after ball milling is 50-150 microns; the ball mill used in this process is produced by Nanjing University Instrument Factory The QM-BP planetary ball mill;
(5)球磨混匀后的混合物进行真空干燥，形成干燥混合粉体；(5) The mixture after ball milling and mixing is vacuum-dried to form a dry mixed powder;
(6)将混合粉体装入模压成型模具中，热压成型，成型温度为110℃，成型压力为20MPa，保温保压时间为100min，得到高导热相变复合材料。(6) Put the mixed powder into a compression molding mold, and hot press molding, the molding temperature is 110°C, the molding pressure is 20MPa, the heat preservation and pressure holding time is 100min, and a high thermal conductivity phase change composite material is obtained.
所制备的复合材料性能如下： The properties of the prepared composite material are as follows:
密度：0.87g/cm3；热导率：0.94W/m K。Density: 0.87g/cm3 ; thermal conductivity: 0.94W/m K.
实施例2：具体制备过程如下： Embodiment 2: The specific preparation process is as follows:
(1)，(2)和(5)同实施例1；(1), (2) and (5) are with embodiment 1;
(3)膨胀石墨粉末、粉末状高密度聚乙烯、粉末状相变微胶囊进行按照质量比10:40:50进行配料；所选用样品同实施例1；(3) Expanded graphite powder, powdery high-density polyethylene, and powdery phase-change microcapsules are batched according to the mass ratio of 10:40:50; the selected samples are the same as in Example 1;
(4)将配好的混合物装入球磨机中，加入无水乙醇，进行湿法球磨，时间为180min，球磨后混合物的粒径为50-200微米；选用球磨机同实施例1；(4) Pack the prepared mixture into a ball mill, add absolute ethanol, and carry out wet ball milling for 180 minutes. The particle diameter of the mixture after ball milling is 50-200 microns; the ball mill is the same as in Example 1;
(6)将混合粉体装入模压成型模具中，热压成型，成型温度为100℃，成型压力为15MPa，保温保压时间为130min，得到高导热相变复合材料。(6) Put the mixed powder into a compression molding mold, hot press molding, the molding temperature is 100°C, the molding pressure is 15MPa, the heat preservation and pressure holding time is 130min, and a high thermal conductivity phase change composite material is obtained.
所制备的复合材料性能如下： The properties of the prepared composite material are as follows:
密度：0.92g/cm3；热导率：4.59W/m K。Density: 0.92g/cm3 ; thermal conductivity: 4.59W/m K.
实施例3：具体制备过程如下： Embodiment 3: the specific preparation process is as follows:
(1)，(2)和(5)同实施例1；(1), (2) and (5) are with embodiment 1;
(3)膨胀石墨粉末、粉末状高密度聚乙烯、粉末状相变微胶囊进行按照质量比15:40:45进行配料；所选用样品同实施例1；(3) Expanded graphite powder, powdery high-density polyethylene, and powdery phase-change microcapsules are batched according to the mass ratio of 15:40:45; the selected samples are the same as in Example 1;
(4)将配好的混合物装入球磨机中，加入无水乙醇，进行湿法球磨，时间为200min，球磨后混合物的粒径为80-220微米；选用球磨机同实施例1；(4) the prepared mixture is packed into a ball mill, add absolute ethanol, and carry out wet ball milling, the time is 200min, the particle diameter of the mixture after ball milling is 80-220 microns; select the ball mill for use with embodiment 1;
(6)将混合粉体装入模压成型模具中，热压成型，成型温度为120℃，成型压力为25MPa，保温保压时间为140min，得到高导热相变复合材料。(6) Put the mixed powder into a compression molding mold, hot press molding, the molding temperature is 120°C, the molding pressure is 25MPa, the heat preservation and pressure holding time is 140min, and a high thermal conductivity phase change composite material is obtained.
所制备的复合材料性能如下： The properties of the prepared composite material are as follows:
密度：1.02g/cm3；热导率：6.01W/m K。Density: 1.02g/cm3 ; thermal conductivity: 6.01W/m K.
实施例4： Example 4:
(1)，(2)和(5)同实施例1；(1), (2) and (5) are with embodiment 1;
(3)膨胀石墨粉末、粉末状高密度聚乙烯、粉末状相变微胶囊进行按照质量比20:35:45进行配料；所选用样品同实施例1；(3) Expanded graphite powder, powdery high-density polyethylene, and powdery phase-change microcapsules are batched according to the mass ratio of 20:35:45; the selected samples are the same as in Example 1;
(4)将配好的混合物装入球磨机中，加入无水乙醇，进行湿法球磨，时间为180min，球磨后混合物的粒径为90-250微米；选用球磨机同实施例1；(4) The prepared mixture is packed into a ball mill, added absolute ethanol, and carried out wet ball milling, the time is 180min, and the particle diameter of the mixture after ball milling is 90-250 microns; the ball mill is the same as in Example 1;
(6)将混合粉体装入模压成型模具中，热压成型，成型温度为110℃，成型压力为30MPa，保温保压时间为120min，得到高导热相变复合材料。(6) Put the mixed powder into a compression molding mold, hot press molding, the molding temperature is 110°C, the molding pressure is 30MPa, the heat preservation and pressure holding time is 120min, and a high thermal conductivity phase change composite material is obtained.
所制备的复合材料性能如下： The properties of the prepared composite material are as follows:
密度：1.0g/cm3；热导率：9.9W/m K。Density: 1.0g/cm3 ; thermal conductivity: 9.9W/m K.
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| CN2013100934948ACN103183862A (en) | 2013-03-22 | 2013-03-22 | High-thermal-conductivity phase-change composite material and preparation process thereof |
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| WD01 | Invention patent application deemed withdrawn after publication | Application publication date:20130703 |