水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能

程岩; 王诏田; 罗洪杰; 吴林丽; 陈曦平; 姜昊

水溶性锆杂化硅树脂浸润剂提高玄武岩纤维的耐热性能

程岩¹,
王诏田¹,
罗洪杰^{1, 2, ,},
吴林丽¹,
陈曦平¹,
姜昊³

1.
东北大学　冶金学院, 辽宁沈阳 110819
2.
教育部材料先进制备技术工程研究中心, 辽宁沈阳 110819
3.
抚顺天成环保科技有限公司辽宁抚顺 113001

基金项目: 国家自然科学基金资助项目(51874093)

详细信息

通讯作者:
罗洪杰，教授，博士生导师，研究方向为多孔材料制备与固废回收　E-mail：neuhjluo@sina.com

中图分类号: 文献标志码:A
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- 被引次数: 0
出版历程
- 收稿日期: 2022-01-25
- 录用日期: 2022-04-19
- 修回日期: 2022-04-09
- 网络出版日期: 2022-05-11

Water-soluble zirconium hybrid silicone resin sizing for improvement heat resistance of basalt fibre

1.
School of Metallurgy, Northeastern University, Shenyang, Liaoning 110819, China
2.
Engineering Research Center of Ministry of Education for Advance Materials Preparation Technology, Shenyang, Liaoning 110819, China
3.
Tiancheng Environmental Protection Technology Co., Ltd, Fushun, Liaoning 113001, China

摘要

摘要: 现有玄武岩纤维制成的高温烟气滤袋工作温度为280℃，难以在300℃甚至更高的温度下长期工作。为了提高玄武岩纤维的耐热性能，本研究合成了一种水溶性锆杂化硅树脂浸润剂，并用于玄武岩纤维表面改性。用FTIR、TG-DSC、SEM、AFM、DCA及拉伸实验对锆杂化硅树脂及改性纤维进行了微观结构和性能表征。结果表明：锆杂化硅树脂的初始热分解温度为320~360℃；浸润后的玄武岩纤维表面包裹着一层致密、均匀的硅树脂膜，这层膜增大了纤维表面的粗糙度和表面积，提高了纤维的表面能，改变了纤维的表面结构，修复了纤维的表面微缺陷；力学测试表明：浸润后的纤维在300℃热处理2 h后，最优断裂强力值为376 N，强力保持率91.30%，断裂伸长率为2.64%，优于未被浸润纤维(287 N、69.24%、1.93%)的相关性能。因此，锆杂化硅树脂浸润剂可显著提高玄武岩纤维的耐热性能。
- 玄武岩纤维 /
- 锆杂化硅树脂 /
- 浸润剂 /
- 力学性能 /
- 耐热性能
Abstract: The working temperature of the existing high-temperature basalt fibre filter bag is 280℃, they are difficult to work for a long time when the temperature is above 300℃. In order to improve the heat resistance of basalt fibres. In this paper, a kind of water-soluble zirconium hybrid silicone resin sizing agent was synthesized and used for basalt fibre surface modification. Microstructure and properties of zirconium hybrid silicone resin and modified fibers were characterized by FTIR, TG-DSC, SEM, AFM, DCA and tensile test. The results show the decompose temperature of zirconium hybrid silicone resin are 310~360℃. The surfaces of the sized fibres are coated by dense and uniform silicone resin films. These films increase the surface roughness and surface areas of the fibre surfaces, improve the surface energies, change the surface morphologies, repair the surface micro defects. The mechanical tests show that after heat treatment of 2 h at 300℃, the breaking force of optimum sample is 376 N, the force retention rate is 91.30%, and the breaking elongation is 2.64%, which are better than the related performance of uncoated fibre(287 N、69.24%、1.93%). Therefore, the zirconium hybrid silicone sizing agent could significantly improve the heat resistance of basalt fibre.
- Basalt fibre /
- zirconium hybrid silicone resin /
- sizing /
- mechanical properties /
- heat resistance

HTML全文

图 1 水溶性锆杂化硅树脂合成图

Figure 1. Synthesis scheme of water-soluble zirconium hybrid silicone resin

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图 2 锆杂化硅树脂(Zr-SR)的FTIR图谱

Figure 2. FTIR spectra of zirconium hybrid silicone resin (Zr-SR)

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图 3 Zr-SR的TG曲线(a)和DSC曲线(b)

Figure 3. TG curves (a) and DSC curves (b)of Zr-SR

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图 5 BF和Zr-SR/BF-1~Zr-SR/BF-5的AFM图

Figure 5. AFM morphologies of basalt fibre BF and Zr-SR/BF-1~Zr-SR/BF-5

BF (a); Zr-SR/BF-1 (b); Zr-SR/BF-2 (c); Zr-SR/BF-3 (d); Zr-SR/BF-4 (e); Zr-SR/BF-5 (f)

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图 6 BF和Zr-SR/BF的表面积值及表面粗糙度值

Figure 6. Surface roughness and surface area values of BF and Zr-SR/BF

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图 7 BF和Zr-SR/BF-4的XPS全谱图(a)；Zr-SR/BF-4的Zr3 d(b)、O1 s(d)和Si2 p(f)，BF的O1 s(c)、Si2 p(e)XPS分谱图Fig 7 XPS spectra of BF and Zr-SR/BF-4 (a); XPS patterns of Zr3 d (b), O1 s(d), Si2 p(f) of Zr-SR/BF-4 and O1 s(c)、Si2 p(e) of BF

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图 8 玄武岩纤维热处理力学性能图：温度-断裂强力图(a)、温度-断裂伸长率(b)、时间-断裂强力(c)

Figure 8. Mechanical properties of basalt fibre after heat treatment: Temperature-breaking force (a); Temperature-breaking elongations (b); Time-breaking force (c)

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图 9 BF和Zr-SR/BF断裂机制图

Figure 9. Fracture mechanism of BF and Zr-SR/BF

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表 1 水溶性锆杂化硅树脂配方

Table 1. Formulas of the water-soluble zirconium hybrid silicone resin

Code	MTES/mol	KH602/mol	ZrOCl₂·8 H₂O/mol	H₂O/mL	CH₃COOH/g	HDMS/mol	Solid Content /wt%
Zr-SR-1	0.020	0.030	0.0005	2	0.6	0.0025	59.67
Zr-SR-2	0.020	0.030	0.0010	2	0.6	0.0025	60.97
Zr-SR-3	0.020	0.030	0.0015	1.75	0.9	0.0025	61.79
Zr-SR-4	0.020	0.030	0.0020	0.5	1	0.0026	67.36
Zr-SR-5	0.020	0.030	0.0025	0.7	1.2	0.0026	69.79

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表 2 25℃时BF及Zr-SR/BF样品测试液体的性能参数

Table 2. Properties of the testing liquids at 25℃ of BF and Zr-SR/BF samples.

Parameters	$ {\gamma _l} $/(mN·m⁻¹)	$ {\gamma _l}^p $/(mN·m⁻¹)	$ {\gamma _l}^d $/(mN·m⁻¹)
H₂O	72.8	51.0	21.8
CH₂I₂	50.8	2.3	48.5
Notes: $ {\gamma _l} $—Surface energy; $ {\gamma _l}^p $—polar component; $ {\gamma _l}^d $—dispersion component of solution

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表 3 BF和Zr-SR/BF样品的接触角及表面能

Table 3. The contact angles and the surface energies of BF and Zr-SR/BF samples.

Sample	Contact angle/(°)		γ_s^p/(mN·m⁻¹)	γ_s^d/(mN·m⁻¹)	γ_s/(mN·m⁻¹)
Sample	H₂O	CH₂I₂	γ_s^p/(mN·m⁻¹)	γ_s^d/(mN·m⁻¹)	γ_s/(mN·m⁻¹)
BF	119	35.9	9.54	22.85	32.39
Zr-SR/BF-1	106.7	29.0	0.95	43.94	44.90
Zr-SR/BF-2	107.8	53.1	0.10	33.80	33.91
Zr-SR/BF-3	110.2	45.5	0.83	36.25	36.25
Zr-SR/BF-4	111.7	32.7	1.88	41.17	43.06
Zr-SR/BF-5	117.9	45.7	2.43	34.27	36.71

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