Preparation of polyvinylpyrrolidone water-based hybrid coating and its sizing treatment of recycled glass fiber
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摘要: 为有效利用回收玻璃纤维，以正硅酸乙酯、偶联剂为前驱体，聚乙烯吡咯烷酮为成膜剂，在酸催化和不添加催化剂条件下，合成了两种聚乙烯吡咯烷酮水性杂化涂剂。利用制备的杂化涂剂分别对回收的玻璃纤维进行上浆处理，并对上浆处理后的回收玻璃纤维的性能进行研究。结果表明：与不添加催化剂条件下制备的杂化涂剂相比，经酸催化条件下制备的杂化涂剂上浆处理后的回收玻纤表面粗糙度更大；酸催化条件与不添加催化剂条件制备的杂化涂剂上浆处理后的回收玻璃纤维的单纤维拉伸强度分别为(
1322.68 ±98.5) MPa、(1093.84 ±53.8) MPa，相比回收玻璃纤维的单纤维拉伸强度分别提高了39.8%和15.6%。利用单纤维碎断法评价回收玻璃纤维与环氧树脂的界面性能表明，经过酸催化条件与不添加催化条件制备的杂化涂剂上浆处理后的回收玻璃纤维制备的单纤维环氧树脂复合材料的界面剪切强度分别为53.5 MPa、35.7 MPa，比未经过上浆处理的回收玻璃纤维的单纤维环氧树脂复合材料的界面剪切强度分别提高了200.5%与100.8%，显示了在酸催化条件下制备的水性杂化涂剂用于回收玻璃纤维具有可行性。Abstract: In order to effectively utilize recycled glass fiber, two polyvinylpyrrolidone water-based hybrid coatings were synthesized under acid catalysis and without adding catalyst using ethyl orthosilicate and coupling agent as precursors and polyvinylpyrrolidone as film-forming agent. The recycled glass fibers were sized separately using the prepared hybrid coatings. The results show that the surface roughness of the recycled glass fibers after the sizing treatment of the hybrid coatings prepared under acid-catalyzed conditions is greater compared with that of the hybrid coatings prepared under the condition of no added catalyst. The single-fiber tensile strengths of the recycled glass fibers after sizing treatment of the hybrid coatings prepared under acid-catalyzed conditions and conditions without added catalysts are (1322.68 ±98.5) MPa and (1093.84 ±53.8) MPa, which are increased by 39.8% and 15.6%, compared with the single-fiber tensile strengths of the recycled glass fibers. The interfacial properties of recycled glass fiber and epoxy resin were evaluated by the single fiber fragmentation method. The results show that the interfacial shear strengths of single fiber epoxy resin composites prepared from recycled glass fiber after hybrid coating sizing treatment under acid catalysis conditions and without adding catalysis conditions are 53.5 MPa and 35.7 MPa, respectively, which are 200.5% and 100.8% higher than those of single fiber epoxy resin composites of recycled glass fiber without sizing treatment. Aqueous hybrid coatings prepared under acid-catalyzed conditions are shown to be feasible for recycling glass fibers.-
Key words:
- hybrid coating /
- polyvinylpyrrolidone /
- recycling /
- glass fiber /
- interfacial shear strength /
- composite material
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图 1 Sizing agent (Acid)杂化涂剂制备流程
Figure 1. Sizing agent (Acid) hybrid coating preparation process
TEOS—Ethyl orthosilicate; KH550—γ-aminopropyl triethoxysilane; PTSA—p-toluenesulfonic acid; PVP—Polyvinylpyrrolidone
图 2 Sizing agent (Catalyst-free)杂化涂剂制备流程
Figure 2. Sizing agent (Catalyst-free) hybrid coating preparation process
图 3 回收玻纤(GF)杂化涂剂改性示意图
Figure 3. Schematic diagram of modified recycled glass fiber (GF)hybrid coating
图 4 单纤维复合材料试样图
Figure 4. Sample diagram of single fiber composite material
EP—Epoxy resin
图 5 单纤维复合材料单丝断裂试验装置
Figure 5. Single fiber composite material single fiber fracture test device
图 7 杂化涂剂固化后SEM图像：(a) Sizing agent (Acid) 断面； (b) Sizing agent (Catalyst-free)断面
Figure 7. SEM images of hybrid coating cured: (a) Sizing agent (Acid) cross-section; (b) Sizing agent (Catalyst-free) cross-section
图 8 杂化涂剂的TEM图像：((a), (a')) Sizing agent (Acid)；((b), (b')) Sizing agent (Catalyst-free)
Figure 8. TEM images of hybrid coating: ((a), (a')) Sizing agent (Acid); ((b), (b')) Sizing agent (Catalyst-free)
图 9 PVP、Sizing agent (Acid)与Sizing agent (Catalyst-free)的红外图谱(a)及其局部区域放大图(b)
Figure 9. Infrared spectra (a) and enlarged view (b) of PVP, Sizing agent (Acid) and Sizing agent (Catalyst-free)
图 11 不同玻纤试样的SEM图像：((a), (a')) 回收玻璃纤维(RGF)；((b), (b')) 酸化涂剂处理的回收玻璃纤维(ARGF)；((c), (c')) 无酸涂剂处理的回收玻璃纤维(FRGF)
Figure 11. SEM images of different glass fiber samples: ((a), (a')) Recycled glass fiber (RGF); ((b), (b')) Acid-coated recycled glass fibers (ARGF); ((c), (c')) Recycled glass fibers treated with acid-free coatings (FRGF)
图 12 不同试样中EDS元素分布图：(a) RGF；(b) ARGF；(c) FRGF
Figure 12. Distribution of EDS elements in different samples: (a) RGF; (b) ARGF; (c) FRGF
图 13 不同杂化涂剂处理的玻纤表面AFM图像：(a) RGF；(b) ARGF；(c) FRGF
Figure 13. AFM images of glass fiber surfaces treated with different hybrid coatings: (a) RGF; (b) ARGF; (c) FRGF
图 14 RGF、ARGF、FRGF的表面粗糙度：(a)平均粗糙度Ra；(b)最大粗糙度Rmax
Figure 14. Surface roughness of RGF, ARGF and FRGF: (a) Average roughness Ra; (b) Maximum roughness Rmax
图 15 Sizing agent (Acid)、Sizing agent (Catalyst-free)杂化涂剂、RGF及上浆改性玻纤的红外图谱
Figure 15. Infrared spectra of Sizing agent (Acid), Sizing agent (Catalyst-free) hybrid coating, RGF and sizing modified glass fiber
图 16 不同玻纤试样的单丝强度Weibull分布(a)、单丝拉伸强度(b)、代表性应力-应变曲线(c)
Figure 16. Single filament strength Weibull distribution (a), single filament tensile strength (b), representative stress-strain curves (c) of different glass fiber samples
R2—Coefficient of determination in the Weber distribution; F—Minimum mean square error fracture probability; σ—Measured tensile strength of the fibers
图 17 (a)玻纤单丝平均断裂长度；(b)玻纤环氧树脂单纤维复合材料界面剪切强度
Figure 17. (a) Average breaking length of glass fiber monofilament; (b) Interfacial shear strength of glass fiber epoxy resin single fiber composites
图 18 RGF (a)、ARGF (b)与FRGF (c)在环氧树脂基体中达到临界断裂强度的代表性偏光显微镜照片
Figure 18. Polarized light microscope photos of RGF (a), ARGF (b) and FRGF (c) reaching critical fracture strength in epoxy resin matrix
图 19 复合材料的拉伸断裂截面SEM图像：(a) RGF/EP；(b) ARGF/EP；(c) FRGF/EP
Figure 19. SEM images of tensile fracture cross-sections of composite materials: (a) RGF/EP; (b) ARGF/EP; (c) FRGF/EP
表 1 不同玻纤试样的单丝拉伸强度、Weibull参数及界面剪切强度评价相关结果
Table 1. Results related to the evaluation of monofilament tensile strength, Weibull parameters and interfacial shear strength of different glass fiber specimens
Sample $ {\sigma }_{{\mathrm{f}}} $/MPa $ {d}_{{\mathrm{f}}} $/μm m $ \bar{l} $/μm $ l\mathrm{_c} $/μm $ {\tau }_{{\mathrm{IFSS}}} $/MPa RGF 946.43 14 4.57 594.28 792.37 17.79 ARGF 1322.68 15 4.86 321.32 428.43 53.46 FRGF 1093.84 15 5.67 347.89 463.85 35.73 Notes: $ {\sigma }_{{\mathrm{f}}} $—Average tensile strength of glass fiber at gauge length; $ {d}_{{\mathrm{f}}} $—Glass fiber diameter; m—Weibull shape parameter; $ \stackrel{-}{l} $—Average length of glass fiber in fracture test; $ {l}_{{\mathrm{c}}} $—Critical breaking length of glass fiber; $ {\tau }_{{\mathrm{IFSS}}} $—Interface shear strength. 
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