非抄造型复合云母板制备工艺研究及其机理分析
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摘要
云母以其优异的电气绝缘性能广泛用于电工绝缘材料行业,随着大鳞片云母资源的日益枯竭,云母工业通常将碎云母进行水力破碎后抄造成云母纸,以实现碎云母资源的综合利用,但云母纸强度较低,往往需要加入胶粘剂和补强材料将多层云母纸进行复合制成云母板等产品用于电气绝缘行业,从而使得工艺流程较为复杂,而溶剂型绝缘胶粘剂的加入,易在生产过程中排放有毒有害的有机气体,存在环境污染、人员健康威胁等相关问题,同时,由于细粒级云母(<74μ m)无法用于云母纸的抄造,造成云母资源浪费,因此,开发环保型绝缘胶粘剂,改善现有云母板生产工艺流程是当前云母电工绝缘材料行业的发展方向。
针对上述问题,本文提出了以水性环氧绝缘胶粘剂取代现有的溶剂型环氧绝缘胶粘剂,并采用非抄造一次成型技术,不经云母纸的抄造,直接制备复合云母板的新工艺。水性环氧绝缘胶粘剂以水为溶剂,对基材有良好的渗透性和粘结力,安全无毒,经固化交联后,水性环氧树脂具有力学强度高、附着粘结能力强、良好的化学稳定性以及优异的电气绝缘性能,完全满足云母绝缘行业的要求；非抄造成型技术是指不经过云母纸的抄取,直接将混胶好的云母浆料经沉降预成型烘干成云母坯料后热压固化成云母板,工艺流程简单,同时可以利用细粒级云母填充粗粒级云母间的空隙,增强复合云母板的致密程度,解决细粒级云母的浪费问题,提高云母资源利用率。通过大量的试验研究,确定了云母浆料制备工艺、水性环氧绝缘胶粘剂合成及混胶工艺、预成型热压固化工艺,获得了一套较为完整的制备工艺流程,提高非抄造型复合云母板的性能指标,使其满足工业标准。具体结果如下：
1.以混合云母料作为复合云母板的制备原料,通过水力分级和超声波剥片除去细粒级云母(<74μ m)中的石英等杂质,提高其径厚比,与粗粒级云母(>74μ m)进行合理级配,以粗粒级云母为骨架,细粒级云母进行填充,并采用硅烷偶联剂改性云母浆料,提高其与水性环氧树脂的吸附和包裹作用,改善复合材料的电气绝缘性能和耐水性,有效增强了非抄造型复合云母板的性能；
2.根据云母绝缘材料要求,采用聚乙二醇(PEG2000)、苯酐(PA)和顺丁烯二酸酐(MA)复合改性环氧树脂,引入羧基基团,使其具有亲水性,聚乙二醇(PEG2000)改善环氧树脂柔韧性和亲水性,苯酐(PA)由于其结构中含有苯环,能够提高水性环氧树脂的耐热性和耐水性,顺丁烯二酸酐(MA)含有活泼双键,提高固化交联密度,增强复合云母板抗弯强度,并以高度甲醚化的氨基树脂5747作为固化剂,该固化剂含交联活性基团多,有效提高了水性环氧绝缘胶粘剂的成膜性能,降低其吸水率,并确定了最佳的混胶工艺参数,进一步提高非抄造型复合云母板的性能；
3.通过沉降工艺、抽滤工艺和烘干工艺获得了结构较为紧密的复合云母板坯料,采用分步热压成型工艺,包括升温排气阶段,热压固化阶段和保压冷却阶段,解决了排气问题,并确定了最佳热压固化工艺参数。整套工艺的完成有效提高了非抄造型复合云母板的性能,其抗弯强度由165.03N/mm2提高至245.79N/mm2,介电强度由21.96KV/mm提高至28.05KV/mm,分别提升了32.9%和21.7%,吸水率由0.72%下降至0.43%,下降40.3%。经各项性能测试表明,该非抄造型复合云母板在外观、层间结构、机械性能、电气绝缘性能等方而基本达到工业标准,具有良好的工业应用前景。
4.探讨了非抄造型复合云母板制备过程中所涉及的级配增强机理、界面作用机理和水性环氧固化机理,解释了复合材料强度变化的原因,为进一步完善该工艺提供一定的理论基础。
非抄造型复合云母板制备工艺的研究和完成,解决了目前云母电工绝缘材料中存在的相关问题,实现了细粒级云母的重新再利用,提高了云母资源利用率约5%-8%,降低VOC排放,改善了环境污染,对促进我国云母电工绝缘材料的发展,提升云母绝缘材料技术水平,调整产品结构都将起着积极的作用。
Mica widely used in electrical insulation materials industry because of its excellent electrical insulating properties. With the exhausting of large scale mica resource, mica flake is used to producing mica paper by hydraulic crushing in mica insulation industry, and achieve the comprehensive utilization of mica flake. Because low strength of the mica paper, the solvent type adhesive and reinforcing materials is needed when producing the multilayer mica composite insulation materials. Thereby making the process more complicated, and the emission of toxic and hazardous organic gases during the process, this will cause the environmental contamination and personnel health threats and other related issues. Meanwhile, due to the fine mica (<74μm) can not be used for papermaking, caused the waste of mica resources, therefore, the development of environmentally friendly insulation adhesive and improve the existing the mica plate production process is the sustainable development direction of the current mica electrical insulation materials industry.
In order to solve such problems, the preparation of composite mica plate molding technology without papermaking and solvent-based insulation adhesive is introduced. Waterborne epoxy is used as insulation adhesive with the solvent of water; it is safe and non-toxic with good permeability and bond strength for the most materials. After curing crosslinkable, waterborne epoxy resin is fully meet the requirements of the mica insulation industry with a high mechanical strength, strong adhesion bonding capacity, a good chemical stability as well as excellent electrical insulating properties. Non papermaking technology is a new direct molding process. Mixing the mica slurry with the adhesive and preformed by settlement, then the mica composite plate material is directly obtained by hot press curing. The new process is more convenient, and the fine mica can be used to filling the gap between the coarse-grained mica. The densification of mica composite plate is enhanced and the utilization of mica resources is improved. Through extensive experimental research, a complete preparation process is obtained, and specific results are as follow:
1. The raw material of mica composite plate is a kind of mixed mica. After comminuting, the quartz and other impurities in fine-grade mica (<74μm) is removed by hydraulic classification, and the ratio of diameter to thickness is improved by ultrasonic peeling. A reasonable gradation is accomplished, the coarse-grained mica(>74μm) as the skeleton and the fine-grade mica (<74μm) is for filling. In order to improve the adsorption of waterborne epoxy resin with mica slurry, silane coupling agent is introduced to modify the mica particle;
2. According to the requirements of the mica insulation materials, the polyethylene glycol (PEG2000), phthalic anhydride (PA) and maleic anhydride (MA) are used to modify epoxy resin, the carboxyl groups is grafted and make epoxy resin hydrophilic. The polyethylene glycol (PEG2000) is used to improve the flexibility and hydrophilic of epoxy resin, phthalic anhydride (PA) containing a benzene ring in its structure, it is possible to improve the heat resistance and water resistance of the aqueous epoxy resin, maleic acid anhydride (MA) containing a reactive double bond, that can be improving the curing crosslinking density and enhancing the flexural strength of the mica composite plate. Considering the performance and water absorption of the aqueous epoxy insulating adhesive film-forming, highly methylated amino resin5747containing more cross-linking reactive groups is be chosen as the curing agent. In order to improve the performance of non papermaking mica composite plate, the mixing binder process is optimized.
3. The closely structure composite mica blank is obtained after settling, filtering and drying. The program of hot forming process is introduced including heating up and the exhaust stage, the hot pressing and curing stage and holding pressure and cooling stage. The best hot curing process parameter is determined. The performance of the non-papermaking mica composite plate is improved by the completion of the process. The flexural strength of this product is increased from165.03N/mm2to245.79N/mm2, and also of the dielectric strength from21.96KV/mm to28.05KV/mm, all promoted32.9%and21.7%respectively, the water absorption decreased by0.72%to0.43%, a decrease of40.3%. The performance tests indicate that non papermaking mica composite plate is achieve the industry standard basically in appearance, layer structure, mechanical properties, electrical insulation performance, only the high temperature resistance somewhat less than the index. These results illustrate that the composite material have certain industrial applications prospects.
4. The gradation enhancement mechanism, the interface mechanism and the waterborne epoxy curing mechanism is discussed. Explaining the reason of the strength improvement for the composite material, and providing a theoretical basis for the future.
The completion of non papermaking mica composite plate solves the related issues in mica electrical insulation materials and increases the utilization of mica resource. The new process will play an active role to enhance the technical level of mica insulation materials and promote the development of mica electrical insulation industry.
针对上述问题,本文提出了以水性环氧绝缘胶粘剂取代现有的溶剂型环氧绝缘胶粘剂,并采用非抄造一次成型技术,不经云母纸的抄造,直接制备复合云母板的新工艺。水性环氧绝缘胶粘剂以水为溶剂,对基材有良好的渗透性和粘结力,安全无毒,经固化交联后,水性环氧树脂具有力学强度高、附着粘结能力强、良好的化学稳定性以及优异的电气绝缘性能,完全满足云母绝缘行业的要求；非抄造成型技术是指不经过云母纸的抄取,直接将混胶好的云母浆料经沉降预成型烘干成云母坯料后热压固化成云母板,工艺流程简单,同时可以利用细粒级云母填充粗粒级云母间的空隙,增强复合云母板的致密程度,解决细粒级云母的浪费问题,提高云母资源利用率。通过大量的试验研究,确定了云母浆料制备工艺、水性环氧绝缘胶粘剂合成及混胶工艺、预成型热压固化工艺,获得了一套较为完整的制备工艺流程,提高非抄造型复合云母板的性能指标,使其满足工业标准。具体结果如下：
1.以混合云母料作为复合云母板的制备原料,通过水力分级和超声波剥片除去细粒级云母(<74μ m)中的石英等杂质,提高其径厚比,与粗粒级云母(>74μ m)进行合理级配,以粗粒级云母为骨架,细粒级云母进行填充,并采用硅烷偶联剂改性云母浆料,提高其与水性环氧树脂的吸附和包裹作用,改善复合材料的电气绝缘性能和耐水性,有效增强了非抄造型复合云母板的性能；
2.根据云母绝缘材料要求,采用聚乙二醇(PEG2000)、苯酐(PA)和顺丁烯二酸酐(MA)复合改性环氧树脂,引入羧基基团,使其具有亲水性,聚乙二醇(PEG2000)改善环氧树脂柔韧性和亲水性,苯酐(PA)由于其结构中含有苯环,能够提高水性环氧树脂的耐热性和耐水性,顺丁烯二酸酐(MA)含有活泼双键,提高固化交联密度,增强复合云母板抗弯强度,并以高度甲醚化的氨基树脂5747作为固化剂,该固化剂含交联活性基团多,有效提高了水性环氧绝缘胶粘剂的成膜性能,降低其吸水率,并确定了最佳的混胶工艺参数,进一步提高非抄造型复合云母板的性能；
3.通过沉降工艺、抽滤工艺和烘干工艺获得了结构较为紧密的复合云母板坯料,采用分步热压成型工艺,包括升温排气阶段,热压固化阶段和保压冷却阶段,解决了排气问题,并确定了最佳热压固化工艺参数。整套工艺的完成有效提高了非抄造型复合云母板的性能,其抗弯强度由165.03N/mm2提高至245.79N/mm2,介电强度由21.96KV/mm提高至28.05KV/mm,分别提升了32.9%和21.7%,吸水率由0.72%下降至0.43%,下降40.3%。经各项性能测试表明,该非抄造型复合云母板在外观、层间结构、机械性能、电气绝缘性能等方而基本达到工业标准,具有良好的工业应用前景。
4.探讨了非抄造型复合云母板制备过程中所涉及的级配增强机理、界面作用机理和水性环氧固化机理,解释了复合材料强度变化的原因,为进一步完善该工艺提供一定的理论基础。
非抄造型复合云母板制备工艺的研究和完成,解决了目前云母电工绝缘材料中存在的相关问题,实现了细粒级云母的重新再利用,提高了云母资源利用率约5%-8%,降低VOC排放,改善了环境污染,对促进我国云母电工绝缘材料的发展,提升云母绝缘材料技术水平,调整产品结构都将起着积极的作用。
Mica widely used in electrical insulation materials industry because of its excellent electrical insulating properties. With the exhausting of large scale mica resource, mica flake is used to producing mica paper by hydraulic crushing in mica insulation industry, and achieve the comprehensive utilization of mica flake. Because low strength of the mica paper, the solvent type adhesive and reinforcing materials is needed when producing the multilayer mica composite insulation materials. Thereby making the process more complicated, and the emission of toxic and hazardous organic gases during the process, this will cause the environmental contamination and personnel health threats and other related issues. Meanwhile, due to the fine mica (<74μm) can not be used for papermaking, caused the waste of mica resources, therefore, the development of environmentally friendly insulation adhesive and improve the existing the mica plate production process is the sustainable development direction of the current mica electrical insulation materials industry.
In order to solve such problems, the preparation of composite mica plate molding technology without papermaking and solvent-based insulation adhesive is introduced. Waterborne epoxy is used as insulation adhesive with the solvent of water; it is safe and non-toxic with good permeability and bond strength for the most materials. After curing crosslinkable, waterborne epoxy resin is fully meet the requirements of the mica insulation industry with a high mechanical strength, strong adhesion bonding capacity, a good chemical stability as well as excellent electrical insulating properties. Non papermaking technology is a new direct molding process. Mixing the mica slurry with the adhesive and preformed by settlement, then the mica composite plate material is directly obtained by hot press curing. The new process is more convenient, and the fine mica can be used to filling the gap between the coarse-grained mica. The densification of mica composite plate is enhanced and the utilization of mica resources is improved. Through extensive experimental research, a complete preparation process is obtained, and specific results are as follow:
1. The raw material of mica composite plate is a kind of mixed mica. After comminuting, the quartz and other impurities in fine-grade mica (<74μm) is removed by hydraulic classification, and the ratio of diameter to thickness is improved by ultrasonic peeling. A reasonable gradation is accomplished, the coarse-grained mica(>74μm) as the skeleton and the fine-grade mica (<74μm) is for filling. In order to improve the adsorption of waterborne epoxy resin with mica slurry, silane coupling agent is introduced to modify the mica particle;
2. According to the requirements of the mica insulation materials, the polyethylene glycol (PEG2000), phthalic anhydride (PA) and maleic anhydride (MA) are used to modify epoxy resin, the carboxyl groups is grafted and make epoxy resin hydrophilic. The polyethylene glycol (PEG2000) is used to improve the flexibility and hydrophilic of epoxy resin, phthalic anhydride (PA) containing a benzene ring in its structure, it is possible to improve the heat resistance and water resistance of the aqueous epoxy resin, maleic acid anhydride (MA) containing a reactive double bond, that can be improving the curing crosslinking density and enhancing the flexural strength of the mica composite plate. Considering the performance and water absorption of the aqueous epoxy insulating adhesive film-forming, highly methylated amino resin5747containing more cross-linking reactive groups is be chosen as the curing agent. In order to improve the performance of non papermaking mica composite plate, the mixing binder process is optimized.
3. The closely structure composite mica blank is obtained after settling, filtering and drying. The program of hot forming process is introduced including heating up and the exhaust stage, the hot pressing and curing stage and holding pressure and cooling stage. The best hot curing process parameter is determined. The performance of the non-papermaking mica composite plate is improved by the completion of the process. The flexural strength of this product is increased from165.03N/mm2to245.79N/mm2, and also of the dielectric strength from21.96KV/mm to28.05KV/mm, all promoted32.9%and21.7%respectively, the water absorption decreased by0.72%to0.43%, a decrease of40.3%. The performance tests indicate that non papermaking mica composite plate is achieve the industry standard basically in appearance, layer structure, mechanical properties, electrical insulation performance, only the high temperature resistance somewhat less than the index. These results illustrate that the composite material have certain industrial applications prospects.
4. The gradation enhancement mechanism, the interface mechanism and the waterborne epoxy curing mechanism is discussed. Explaining the reason of the strength improvement for the composite material, and providing a theoretical basis for the future.
The completion of non papermaking mica composite plate solves the related issues in mica electrical insulation materials and increases the utilization of mica resource. The new process will play an active role to enhance the technical level of mica insulation materials and promote the development of mica electrical insulation industry.
引文
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