基于微孔漂珠的相变微胶囊制备及其对砂浆力学和热性能影响

张家玮; 黄玮; 黄大建; 李旭辉; 马建虎; 郑永

doi:10.13801/j.cnki.fhclxb.20221027.002

基于微孔漂珠的相变微胶囊制备及其对砂浆力学和热性能影响

doi: 10.13801/j.cnki.fhclxb.20221027.002

1.
兰州交通大学　土木工程学院，兰州 730070
2.
兰州交通大学　材料科学与工程学院，兰州 730070
3.
甘肃第三建设集团有限公司，兰州 730030

基金项目: 国家自然科学基金(52068043)；甘肃省建设科技攻关项目(JKR2021-07)；甘肃省教育厅：优秀研究生“创新之星”项目(2022 CXZX-602)；兰州市人才创新创业项目(2018-RC-57；2019-RC-78)

详细信息

通讯作者:
张家玮，博士，教授，博士生导师，研究方向为FRP加固混凝土耐久性、绿色节能建筑　E-mail:zhangjd@mail.lzjtu.cn

中图分类号: TU528；TB333
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出版历程
- 收稿日期: 2022-08-19
- 修回日期: 2022-09-26
- 录用日期: 2022-10-02
- 网络出版日期: 2022-10-28
- 刊出日期: 2023-08-15

Preparation of phase change microcapsules based on microporous fly-ash cenosphere and its effect on the mechanical and thermal properties of mortar

1.
School of Civil Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China
2.
School of Materials Science and Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China
3.
Gansu Third Construction Group CO., LTD., Lanzhou 730030, China

Funds: National Natural Science Foundation of China (52068043); Gansu Province Construction Science and Technology Project (JKR2021-07); Gansu Provincial Department of Education: Excellent Graduate Student' Innovation Star' Project (2022 CXZX-602); Lanzhou Talent Innovation and Entrepreneur Ship Project (2018-RC-57; 2019-RC-78)

摘要

摘要: 为研究基于微孔漂珠的相变微胶囊对砂浆性能的影响，采用真空吸附法，以石蜡为芯材，粉煤灰微孔漂珠为壁材制备复合相变微胶囊，通过等体积代砂法将其加入砂浆中制成相变微胶囊储能砂浆。采用SEM分析复合相变微胶囊的微观形貌，通过DSC和TG表征复合相变微胶囊的热性能，并在此基础上研究复合相变微胶囊的引入对砂浆力学强度及温控性能的影响。结果表明：制备的复合相变微胶囊具有良好的分散性、致密的表面及优异的循环稳定性；复合相变微胶囊的引入使砂浆具备一定的温控性能，当相变微胶囊掺量为30%时，储能砂浆相比基准砂浆峰值温度最高下降2.58℃，峰值温度出现时间延迟90 min；由于漂珠具有良好的力学性能，储能砂浆的强度随微胶囊掺量增加虽有所下降，但仍满足规范要求。微胶囊储能砂浆具有良好的力学性能和优异的温控能力，可应用在建筑中实现控温节能的目的。
- 相变材料 /
- 相变储能砂浆 /
- 微胶囊 /
- 粉煤灰漂珠 /
- 微观结构 /
- 力学性能 /
- 热性能 /
- 温控性能
Abstract: To investigate the effect of phase change microcapsules on the properties of mortar, we reported the high-performance composite phase change microcapsules using the vacuum adsorption method, where fly-ash cenosphere microporous served as a supporting skeleton and paraffin as a latent heat storage unit. The preparation phase change microcapsules were added to the mortar in equal volume sand substitution method to prepare energy storage mortars. The micro-morphology of the composite phase change microcapsules was analyzed by SEM image, and the thermal properties of the composite phase change microcapsules were characterized by DSC and TG. The influence of the introduction of the composite phase change microcapsules on the mechanical strength and temperature control performance of the mortar was studied. The test results show that the prepared composite phase change microcapsules have good dispersion ability, dense surface, and excellent cycle stability. In addition, introducing composite phase change microcapsules gives the mortar a certain temperature control performance. Compared with the blank mortar, the peak temperature of the energy storage mortar with the phase change microcapsules content of 30% decreased by 2.58℃, and the appearance time of the peak temperature was also delayed by 90 min. The mechanical strength of the energy storage mortar decreases slightly with the increase of the microcapsules content, but still meets the standard requirements. The energy storage mortar developed in this study has better mechanical properties and excellent temperature-regulating ability, and it is equally amenable to tempera-ture regulation and building energy conservation.
- phase change materials /
- phase change energy storage mortar /
- microcapsules /
- fly-ash cenosphere /
- microstructure /
- mechanical property /
- thermal performance /
- temperature control performance

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图 1 石蜡DSC曲线

T_c—Peak cooling temperature; ΔH_c—Latent heat of cooling phase transition; T_m—Peak heating temperature; ΔH_m—Latent heat of heating phase transition

Figure 1. DSC curves of paraffin

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图 2 粉煤灰漂珠

Figure 2. Fly-ash cenosphere

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图 3 粉煤灰漂珠XRD图谱

Figure 3. XRD patterns of fly-ash cenosphere

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图 4 “三步法”筛选微孔漂珠

Figure 4. 'Three-step method' to prepare fly-ash micropore cenosphere

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图 5 真空吸附法制备相变微胶囊

Figure 5. Preparation of phase change microcapsules by vacuum adsorption

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图 6 相变微胶囊示意图：(a) 未封装；(b) 封装后

Figure 6. Phase change microcapsule diagram: (a) Unpackaged; (b) Encapsulated

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图 7 相变微胶囊储能砂浆制备

Figure 7. Preparation diagram of phase change microcapsule energy storage mortar

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图 8 基准砂浆和30%掺量相变微胶囊储能砂浆温控性能试验箱

Figure 8. Reference mortar temperature control performance test box and the 30% phase change microcapsule energy storage mortar temperature control performance test box

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图 9 温控性能试验箱尺寸及传感器分布

Figure 9. Temperature control performance test box size and sensor distribution

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图 10 SEM图像：((a), (b)) 粉煤灰漂珠；(c) 微孔漂珠

Figure 10. SEM images: ((a), (b)) Fly-ash cenosphere; (c) Microporous cenosphere

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图 11 SEM图像：(a) 未封装石蜡微胶囊；((b), (c)) 已封装石蜡微胶囊

Figure 11. SEM images: (a) Unpackaged paraffin microcapsules; ((b), (c)) Encapsulated paraffin microcapsules

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图 12 砂浆试件抗折试验图：(a) 基准砂浆试件破坏断面；(b) 相变微胶囊储能砂浆试件破坏断面

Figure 12. Flexural test mortar specimen diagram: (a) Reference mortar specimen failure section; (b) Phase change microcapsule energy storage mortar specimen failure section

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图 13 砂浆抗折强度：(a) 7天；(b) 28天

Figure 13. Mortar flexural strength: (a) 7 days; (b) 28 days

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图 14 砂浆试件抗压试验图：(a) 基准砂浆试件；(b) 相变微胶囊储能砂浆试件

Figure 14. Compressive test of mortar specimen diagram: (a) Benchmark mortar specimen; (b) Phase change microcapsule energy storage mortar specimen

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图 15 砂浆抗压强度：(a) 7天；(b) 28天

Figure 15. Mortar compressive strength: (a) 7 days; (b) 28 days

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图 16 砂浆压折强度比

Figure 16. Mortar compressive strength and flexural strength ratio

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图 17 微胶囊相变循环后质量及潜热损失率

Figure 17. Quality and latent heat loss rate of phase change microcapsule after phase change cycle

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图 18 TG曲线：(a) 石蜡；(b) 相变微胶囊

Figure 18. TG curves: (a) Paraffin; (b) Phase change microcapsules

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图 19 不同相变微胶囊掺量砂浆比热容

Figure 19. Specific heat capacity of mortar of different dosage of phase change microcapsules

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图 20 DSC曲线：(a) SJ-P0砂浆；(b) SJ-P30砂浆；(c)相变微胶囊

Figure 20. DSC curves: (a) SJ-P0 mortar; (b) SJ-P30 mortar; (c) Phase change microcapsules

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图 21 室外温度、湿度及太阳辐射

Figure 21. Outdoor ambient temperature, humidity and solar radiation intensity

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图 22 室外温度、SJ-P0和SJ-P30试验箱内温度

Figure 22. Temperature of outdoor ambient, SJ-P0 and SJ-P30 test box

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图 23 室外湿度、SJ-P0和SJ-P30试验箱内湿度

Figure 23. Humidity of outdoor ambient, SJ-P0 and SJ-P30 test box

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图 24 不同时间段室外温度、SJ-P0和SJ-P30试验箱内温度

Figure 24. Temperature of outdoor, SJ-P0 and SJ-P30 test box in different time period

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表 1 漂珠化学成分

Table 1. Chemical constituents of fly-ash cenosphere wt%

SiO₂	Al₂O₃	Fe₂O₃	K₂O	CaO	MgO	TiO₂	Na₂O	Other
58.9	27.6	5.5	3.1	1.6	1.2	0.9	0.6	0.6

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表 2 微孔漂珠对石蜡的负载率

Table 2. Paraffin adsorption rate of microporous cenosphere

Microporous cenosphere quality/g		Quality of phase change microcapsules after adsorption of paraffin wax/g				Average value/g	Paraffin loading rate/%
20.00		35.72	35.82	35.57		35.70	78.52

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表 3 砂浆配合比

Table 3. Mix proportion of mortar

Sample number	Cement /(kg·m⁻³)	Water/(kg·m⁻³)	Medium sand/(kg·m⁻³)	Phase change microcapsule /(kg·m⁻³)
SJ-P0	450	225	1350.0	0
SJ-P10	450	225	1215.0	42.6
SJ-P15	450	225	1147.5	63.9
SJ-P25	450	225	1012.5	106.5
SJ-P30	450	225	945.0	127.8

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表 4 微胶囊相变循环后质量及潜热

Table 4. Quality and latent heat of phase change microcapsule after phase change cycle

Description of sample	Phase change cycle times
Description of sample	0	30	60	90	120
Latent heat of phase change/(J·g^-1)	60.08	59.77	59.62	59.56	59.55
Quality loss/g	20.00	19.89	19.85	19.82	19.81

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表 5 相变微胶囊储能砂浆降温过程DSC测试结果

Table 5. DSC test results of cooling process of phase change microcapsule energy storage mortar

Sample number	Initial solidification temperature/℃	Phase transition peak temperature/℃	Phase change latent heat /(J·g^-1)
SJ-10	18.44	16.69	5.39
SJ-15	18.39	16.75	8.19
SJ-25	18.97	16.80	14.45
SJ-30	18.86	16.84	18.74

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表 6 相变微胶囊储能砂浆升温过程DSC测试结果

Table 6. DSC test results of heating process of phase change microcapsule energy storage mortar

Sample number	Initial melting temperature /℃	Phase transition peak temperature/℃	Phase change latent heat /(J·g^-1)
SJ-10	19.69	22.64	6.67
SJ-15	19.77	22.73	9.42
SJ-25	20.32	23.27	15.81
SJ-30	20.19	23.19	19.18

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表 7 2021-10-07~2021-10-12试验箱峰值温度和峰值时间差

Table 7. 2021-10-07~2021-10-12 test box peak temperature and peak time difference

Date	Peak high temperature difference value/℃	Time difference of peak high temperature/min	Peak low temperature difference value/℃	Time difference of peak low temperature/min
10-07-10-08	−2.58	60	1.37	90
10-08-10-09	−2.38	40	0.82	10
10-09-10-10	−2.16	30	2.21	20
10-10-10-11	−2.09	70	0.68	10
10-11-10-12	−2.09	70	0.68	10
Note: Peak temperature and peak time difference are SJ-P30 test box minus SJ-P0 test box.

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