聚乙二醇高导热定形相变复合材料的制备及其性能研究

doi:10.11949/0438-1157.20221141

化工学报 ›› 2022, Vol. 73 ›› Issue (12): 5660-5671.DOI: 10.11949/0438-1157.20221141

• 材料化学工程与纳米技术 • 上一篇下一篇

聚乙二醇高导热定形相变复合材料的制备及其性能研究

崔雯琦¹^,²(), 杨曙光¹^,³, 李红周¹, 罗富彬¹()

^1.福建师范大学环境与资源学院，福建福州 350007
^2.福建师范大学环境与资源学院，聚合物资源绿色循环利用教育部工程研究中心，福建福州 350007
^3.福建师范大学环境与资源学院，福建省污染控制与资源循环利用重点实验室，福建福州 350007

收稿日期:2022-08-15 修回日期:2022-10-23 出版日期:2022-12-05 发布日期:2023-01-17
通讯作者: 罗富彬
作者简介:崔雯琦(1999—)，女，硕士研究生， 1992926413@qq.com
基金资助:
泉港石化专项科技项目(2019YJY02);国家自然科学基金青年基金项目(51903049)

Preparation of highly thermally conductive and shape-stabilized polyethylene glycol-based phase change material

Wenqi CUI¹^,²(), Shuguang YANG¹^,³, Hongzhou LI¹, Fubin LUO¹()

^1.College of Environmental and Resources, Fujian Normal University, Fuzhou 350007, Fujian, China
^2.Engineering Research Center of Polymer Green Recycling of Ministry of Education, College of Environmental and Resources, Fujian Normal University, Fuzhou 350007, Fujian, China
^3.Fujian Key Laboratory of Pollution Control & Resource Reuse, College of Environmental and Resources, Fujian Normal University, Fuzhou 350007, Fujian, China

Received:2022-08-15 Revised:2022-10-23 Online:2022-12-05 Published:2023-01-17
Contact: Fubin LUO

摘要/Abstract

摘要：

利用聚乙二醇为相变组分，以氮化硼为导热填料，通过两步法络合聚丙烯酸制备了具有相变稳定性的高导热相变复合材料。系统研究了片状氮化硼以及片状/球形混杂填充对复合材料导热以及相变性能的影响，探讨了相变复合材料的定形机理。结果表明，由于紧密的堆砌结构，片状氮化硼能够有效提升复合材料导热性能。填充60%（质量）的片状氮化硼时，热导率最高达到6.437 W/(m·K)。在混杂填充时，球形氮化硼与片状氮化硼的质量比为1∶3以及1∶6时，可以更加有效提升复合材料的导热性能。热储存实验显示，所制备的复合材料具有良好的热存储能力。此外，由于聚丙烯酸与聚乙二醇形成氢键的络合以及氮化硼的片状物理阻隔作用，复合材料在高温加热条件下具有优异的相变稳定性。

关键词: 复合材料, 相变, 聚合物, 热传导, 氮化硼

Abstract:

Shape-stabilized and highly thermally conductive phase change materials (PCMs) have been prepared based on polyethylene glycol (PEG) and boron nitride (BN). The PCMs are obtained by two-step blending assisted by the complexation of polyacrylic acid (PAA). The thermal conductivity and the stabilization mechanism of the PCMs have been investigated. The results show that the flake-like BN can significant improve the thermal conductivity of the composites. The thermal conductivity of the prepared PCMs can reach to 6.437 W/(m·K) when the mass fraction of BN is 60%. It is also confirmed that when one-third and one-sixth of flake-like BN is replaced by the spherical BN, the composites show an increased thermal conductivity, which suggests that the hybrid fillers has positive effect on the enhancement of thermal conductivity. The experimental results demonstrate that PAA can form hydrogen bond with PEG, which contributes to preventing the leakage of PEG from the matrix when enduring heating. In addition, abundant flake-like BN can act as a solid physical barriers to restrict the molten PEG being escaped from the matrix, resulting the excellent shape preserving property.

Key words: composites, phase change, polymers, heat conduction, boron nitride

中图分类号:

TQ 316.6

崔雯琦, 杨曙光, 李红周, 罗富彬. 聚乙二醇高导热定形相变复合材料的制备及其性能研究[J]. 化工学报, 2022, 73(12): 5660-5671.

Wenqi CUI, Shuguang YANG, Hongzhou LI, Fubin LUO. Preparation of highly thermally conductive and shape-stabilized polyethylene glycol-based phase change material[J]. CIESC Journal, 2022, 73(12): 5660-5671.

图/表 13

表1 所制备复合材料的PEG、PAA以及BN质量比例

Table 1 The mass ratio of PEG， PAA and BN in the composites

Sample	PEG质量/g	PAA质量/g	PEG与PAA的质量比	f-BN质量/g	s-BN质量/g	f-BN与s-BN的质量比
PCM-(PEG₃/PAA₁)-(f-BN₃/s-BN₁)	30.0	10.0	3∶1	45.0	15.0	3∶1
PCM-(PEG₆/PAA₁)-(f-BN₆/s-BN₁)	34.3	5.7	6∶1	51.4	8.6	6∶1
PCM-(PEG₉/PAA₁)-(f-BN₉/s-BN₁)	36.0	4.0	9∶1	54.0	6.0	9∶1
PCM-(PEG₁₂/PAA₁)-(f-BN₁₂/s-BN₁)	36.9	3.1	12∶1	55.4	4.6	12∶1
PCM-(PEG₃/PAA₁)-(f-BN-60)	30.0	10.0	3∶1	60.0	0
PCM-(PEG₆/PAA₁)-(f-BN-60)	34.3	5.7	6∶1	60.0	0
PCM-(PEG₉/PAA₁)-(f-BN-60)	36.0	4.0	9∶1	60.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-60)	36.9	3.1	12∶1	60.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-40)	55.4	4.6	12∶1	40.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-20)	73.8	6.2	12∶1	20.0	0

图1 片状氮化硼(a)和球形氮化硼(b)的SEM图

Fig.1 SEM images of flake-like boron nitride (a) and spherical boron nitride (b)

图2 60%(质量)片状氮化硼填充(a)、片状/球形氮化硼混杂填充(b)和不同含量片状氮化硼填充(c)的相变复合材料热导率

Fig.2 Thermal conductivity of the PCM composites filled with 60%(mass) flake-like boron nitride (a), flake-like/spherical boron nitride hybrids (b) and different content of flake-like boron nitride (c), respectively

图3 片状/球形氮化硼混杂填充相变复合材料扫描电镜图：(a)s-BN∶f-BN=1∶3, (b) s-BN∶f-BN=1∶6, (c) s-BN∶f-BN=1∶9, (d) s-BN∶f-BN=1∶12；复合材料内部结构示意图：(e) s-BN∶f-BN=1∶6, (f) s-BN∶f-BN=1/12

Fig.3 SEM images of PCM composites filled with flake-like/spherical boron nitride hybrids: (a) s-BN∶f-BN=1∶3, (b) s-BN∶f-BN=1∶6, (c) s-BN∶f-BN=1∶9, (d) s-BN∶f-BN=1∶12；Schematic diagram of thermally conductive paths: (e) s-BN∶f-BN=1∶6, (e) s-BN∶f-BN=1∶12

图4 片状氮化硼(a)和片状/球形氮化硼混杂(b)填充相变复合材料的DSC曲线

Fig.4 DSC curves of the PCM composites filled with flake-like boron nitride (a) and flake-like/spherical boron nitride hybrids (b)

表2 片状氮化硼填充相变复合材料相变焓以及相转变温度

Table 2 Phase transformation enthalpy and phase transition temperature of the prepared PCM composites filled with flake-like boron nitride

Sample	T_m/℃	ΔH_m/(J/g)	Theoretical Δ H_m/(J/g)	T_c/℃	ΔH_c/(J/g)	Theoretical Δ H_c/(J/g)
PEG	58.93	141.2		39.48	139.5
PCM-(PEG₃/PAA₁)-(f-BN-60)	53.63	33.91	42.36	—	—	41.85
PCM-(PEG₆/PAA₁)-(f-BN-60)	58.42	40.18	48.41	24.28	37.44	47.83
PCM-(PEG₉/PAA₁)-(f-BN-60)	57.69	50.70	50.83	32.55	49.88	50.22
PCM-(PEG₁₂/PAA₁)-(f-BN-60)	57.93	51.07	52.14	35.84	47.65	51.51
PCM-(PEG₁₂/PAA₁)-(f-BN-40)	56.70	90.94	78.22	30.93	87.45	77.28
PCM-(PEG₁₂/PAA₁)-(f-BN-20)	58.08	119.1	104.21	36.19	119.0	102.95

表3 片状/球形氮化硼（60%）混杂填充PEG/PAA复合材料相变焓以及相转变温度

Table 3 Phase transformation enthalpy and phase transition temperature of the prepared PCM composites filled with flake-like/spherical boron nitride hybrids （60%）

Sample	T_m/℃	Δ H_m/(J/g)	Theoretical Δ H_m/(J/g)	T_c/℃	Δ H_c/(J/g)	Theoretical Δ H_c/(J/g)
PCM-(PEG₃/PAA₁)-(f-BN₃/s-BN₁)	58.51	28.69	42.36	—	—	41.85
PCM-(PEG₆/PAA₁)-(f-BN₆/s-BN₁)	58.83	37.43	48.41	24.56	35.89	47.83
PCM-(PEG₉/PAA₁)-(f-BN₉/s-BN₁)	53.83	32.72	50.83	24.57	32.97	50.22
PCM-(PEG₁₂/PAA₁)-(f-BN₁₂/s-BN₁)	55.34	40.17	52.14	30.28	39.48	51.51

图5 片状氮化硼填充相变复合材料的XRD谱图[(b)为(a)中框线标记部分放大图]

Fig.5 XRD patterns of the PCM composites filled with flake-like boron nitride [(b) is the enlarged view of the zone marked by dotted lines in (a)]

图6 相变复合材料在加热条件下的形状稳定性观察图：(a)样品在长时间加热(100℃)条件下的变化图；(b)样品在80℃下冷热循环的变化图[样品(1)、(2)、(3)和(4)为f-BN含量为60%，PAA与PEG的比值分别为1∶3、1∶6、1∶9、1∶12的复合材料样品，对应PCM-(PEG3/PAA1)-(f-BN-60)、PCM-(PEG6/PAA1)-(f-BN-60)、PCM-(PEG9/PAA1)-(f-BN-60)、PCM-(PEG12/PAA1)-(f-BN-60)，样品(5)为仅添加60%(质量) f-BN的PEG/f-BN复合材料]

Fig.6 The shape stability performance of the prepared PCM composites: (a) digital pictures of the specimens upon heating (100℃); (b) digital pictures of the specimens upon heating and cooling cycles at 80℃ [the specimen codes (1), (2), (3) and (4) represent the PCM composite containing a PAA /PEG ratio of 1∶3, 1∶6, 1∶9, 1∶12, respectively, corresponding to PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG6/PAA1)-(f-BN-60), PCM-(PEG9/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), the specimen code (5) refers to the PEG/f-BN PCM composite]

图7 相变复合材料在加热条件下的形状稳定性观察图: (a)样品在长时间加热(100℃)条件下的变化图;(b)样品在80℃下冷热循环的变化图[样品(6)、(7)和(8)为PAA与PEG的比值为1∶12，f-BN的质量分数分别为20%、40%和60%的复合材料样品，分别对应样品PCM-(PEG12/PAA1)-(f-BN-20)、PCM-(PEG12/PAA1)-(f-BN-40)和PCM-(PEG12/PAA1)-(f-BN-60)]

Fig.7 The shape stability performance of the prepared PCM composites: (a) digital pictures of the specimens upon heating (100℃); (b) digital pictures of the specimens upon heating and cooling cycles at 80℃ [the specimen codes (6), (7) and (8) represent the PCM composite filled with 20%(mass), 40%(mass) and 60%(mass) f-BN respectively, corresponding to PCM-(PEG12/PAA1)-(f-BN-20)，PCM-(PEG12/PAA1)-(f-BN-40) and PCM-(PEG12/PAA1)-(f-BN-60)]

图8 相变复合材料的红外图(a)；相变复合材料的扫描电镜图(b)，其中(1)、(2)、(3)和(4)分别对应样品PCM-(PEG3/PAA1)-(f-BN-60)、PCM-(PEG6/PAA1)-(f-BN-60)、PCM-(PEG9/PAA1)-(f-BN-60)、PCM-(PEG12/PAA1)-(f-BN-60)；相变复合材料定形机理图(c)

Fig.8 FTIR of the PCM composites (a), SEM of the PCM composites (b), where (1), (2), (3) and (4) corresponding to PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG6/PAA1)-(f-BN-60), PCM-(PEG9/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), respectively; shape stabilized mechanism diagram of the PCM composite (c)

表4 文献报道聚乙二醇基导热相变复合材料对比

Table 4 Comparison of polyethylene glycol-based thermally conductive phase change composites reported in literature

编号	填充组分	填料比例	定形以及制备方式	热导率/（W/(m·K))	文献
1	膨胀石墨/改性云母	3.22%(质量)/32.25%(质量)	多孔石墨定形，真空浸渍法	0.56	[34]
2	银纳米线/膨胀蛭石	19.3%(质量)/21.9%(质量)	膨胀蛭石定形，物理共混和浸渍法	0.68	[25]
3	氮化硼/石墨烯	23%(质量)/少量	冰模板自组装氮化硼/石墨烯多孔类气凝胶定形，真空浸渍法	2.36	[29]
4	硅藻土/碳纳米管	36.8%(质量)/3.2%(质量)	硅藻土孔结构定形，浸渍法	1.52	[35]
5	改性二氧化硅/氧化碳纳米管	39.4%(质量)/0.6%(质量)	改性二氧化硅定形，溶胶-凝胶法	0.41	[36]
6	氮化硼/纳米纤维素/壳聚糖	47.4%(质量)/15.8%(质量)/2.4%(质量)	纳米纤维素/壳聚糖界面相互作用定形，界面聚电解质络合纺丝法	4.005	[37]
7	二氧化硅/石墨	10%(质量)/6%(质量)	二氧化硅网状分子结构定形，溶胶-凝胶法和浸渍法	1.867	[38]
8	聚丙烯酰胺	40%(质量)	聚丙烯酰胺三维网络结构定形,化学交联法	0.375	[39]
9	氮化硼/聚丙烯酸	60%(质量)/3.1%(质量)	片状氮化硼阻隔及聚丙烯酸氢键络合，熔融共混浇筑法	6.437	本文

图9 样品E51/BN、PEG/PAA、PCM-(PEG3/PAA1)-(f-BN-60)和PCM-(PEG12/PAA1)-(f-BN-60)加热条件下表面温度变化曲线(a)；加热台储能示意图(b)；样品在加热时的红外热成像图(c)，(T-1)，(T-2)，(T-3)，(T-4)分别对应样品PCM-(PEG3/PAA1)-(f-BN-60)、PCM-(PEG12/PAA1)-(f-BN-60)、E51/BN，PEG/PAA

Fig.9 Surface temperature variation curves of E51/BN, PEG/PAA, PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60) samples recorded by an infrared imaging devices upon heating (a); the diagram of the testing experiment (b); infrared thermal imaging of four samples upon heating (c); where (T-1), (T-2), (T-3), (T-4) are corresponding to PEG/PAA, PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), E51/BN, PEG/PAA, respectively

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聚乙二醇高导热定形相变复合材料的制备及其性能研究

Preparation of highly thermally conductive and shape-stabilized polyethylene glycol-based phase change material

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