CN117341300A - 一种自粘聚酰亚胺云母带及其生产工艺 - Google Patents
一种自粘聚酰亚胺云母带及其生产工艺 Download PDFInfo
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- CN117341300A CN117341300A CN202311341396.1A CN202311341396A CN117341300A CN 117341300 A CN117341300 A CN 117341300A CN 202311341396 A CN202311341396 A CN 202311341396A CN 117341300 A CN117341300 A CN 117341300A
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- Prior art keywords
- layer
- adhesive
- polyimide
- mica
- polyimide film
- Prior art date
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 89
- 239000010445 mica Substances 0.000 title claims abstract description 77
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 77
- 239000004642 Polyimide Substances 0.000 title claims abstract description 34
- 239000000853 adhesive Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 239000010410 layer Substances 0.000 claims abstract description 96
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012790 adhesive layer Substances 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 32
- 239000004744 fabric Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims description 31
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 22
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 17
- 230000001070 adhesive effect Effects 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
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- 238000000576 coating method Methods 0.000 claims description 9
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 9
- VSIKJPJINIDELZ-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octakis-phenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)O[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 VSIKJPJINIDELZ-UHFFFAOYSA-N 0.000 claims description 8
- GPXCORHXFPYJEH-UHFFFAOYSA-N 3-[[3-aminopropyl(dimethyl)silyl]oxy-dimethylsilyl]propan-1-amine Chemical compound NCCC[Si](C)(C)O[Si](C)(C)CCCN GPXCORHXFPYJEH-UHFFFAOYSA-N 0.000 claims description 8
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 8
- HLFXUXNJUQPIMK-UHFFFAOYSA-N hydroxysilane tetramethylazanium Chemical compound [SiH3]O.C[N+](C)(C)C HLFXUXNJUQPIMK-UHFFFAOYSA-N 0.000 claims description 8
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical compound [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 claims description 3
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
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- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 description 2
- BDGLHSZEDTUSJC-UHFFFAOYSA-N N'-[3-[methyl(silyloxy)silyl]propyl]ethane-1,2-diamine Chemical compound C[SiH](CCCNCCN)O[SiH3] BDGLHSZEDTUSJC-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 2
- 230000003137 locomotive effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
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Abstract
本发明公开了一种自粘聚酰亚胺云母带及其生产工艺,涉及绝缘材料技术领域。本发明生产的云母带包括云母纸层,云母纸层一侧设置聚酰亚胺薄膜层、另一侧设置有无碱玻璃布层,云母纸层与聚酰亚胺薄膜层通过第一胶粘剂层复合,云母纸层与无碱玻璃布层通过第二胶粘剂层复合;聚酰亚胺薄膜层由二胺、二酐以及改性氧化铝混合反应制得;本申请制备的聚酰亚胺薄膜具有耐电晕、粘结性能强以及耐老化效果好的特点,本申请制备的聚酰亚胺薄膜以及无碱玻璃布层作为增强层、与云母纸层复合制备云母带,得到的云母带应用在变频电机中具有优良的绝缘稳定性。
Description
技术领域
本发明涉及绝缘材料技术领域,具体涉及一种自粘聚酰亚胺云母带及其生产工艺。
背景技术
随着电力电子技术的发展,大功率高速开关器件广泛应用于高速机车的变频调速系统中,变频电机具有控制方便、节能等优势,已在高速铁路、舰船、家电等众多领域得到了广泛应用。其中在高速动车组等普通采用变频调速交流传动系统,变频调速牵引电机是交流传动电力机车的关键部件之一,其性能直接影响到高速动车组运行的稳定性和可靠性。变频调速牵引电机输出的电压具有上升沿陡、频率高等特点,致使牵引电机绝缘长期承受高频陡脉冲电应力,导致绕组端部过电压产生很强的电场;另一方面,电机绝缘系统还承受热、潮气以及频繁机械振动等各种环境应力,加速了电机绝缘的老化速率。
固体材料的介电强度是衡量其绝缘性能的一个重要参数,固体电介质在电、热等应力作用下导致的绝缘击穿将产生永久性的绝缘破坏,使电气设备或电子元件的使用寿命终结。聚酰亚胺是一类主链中含有酰亚胺环结构的高性能聚合物。聚酰亚胺薄膜由于具有优异的综合性能,包括耐热性、机械性能、尺寸稳定性及电气绝缘性能,作为牵引电机定子匝间绝缘和对地绝缘的基础绝缘材料在变频调速牵引电机中得到了广泛应用。聚酰亚胺分子链上具有π-π、π-p等共轭体系及醚键、杂环产生的偶极吸引力,使化学键具有较强的稳定性。然而,聚酰亚胺薄膜在服役过程中受到光、电、热、机械、化学腐蚀等因素的作用会逐渐老化降解,分子链断裂使电气强度降低而导致绝缘击穿,对牵引电机的运行带来潜在危险。
发明内容
本发明的目的在于提供一种自粘聚酰亚胺云母带及其生产工艺,解决以下技术问题:
现有的云母带使用的聚酰亚胺薄膜在受到老化降解后,聚酰亚胺分子链断裂导致绝缘材料被击穿。
本发明的目的可以通过以下技术方案实现:
一种自粘聚酰亚胺云母带,所述云母带包括云母纸层,所述云母纸层一侧设置聚酰亚胺薄膜层、另一侧设置有无碱玻璃布层,所述云母纸层与聚酰亚胺薄膜层通过第一胶粘剂层复合,所述云母纸层与无碱玻璃布层通过第二胶粘剂层复合;
所述聚酰亚胺薄膜层的制备方法包括如下步骤:
S1:氮气氛围中,将纳米氧化铝、N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入偏苯三酸酐,分散均匀,加入二月桂酸二丁基锡,控制温度110-120℃,搅拌条件下保温9-12h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将八甲基环四硅氧烷、八苯基环四硅氧烷、1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度90-100℃,加入四甲基铵硅烷醇,保温反应24-36h,控制温度160-165℃,保温0.5-1h,控制温度100-110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将N,N′-二甲基乙酰胺、均苯四甲酸二酐加入反应釜B中,分散均匀,加入4,4′-二氨基二苯醚,控制温度0-5℃,搅拌条件下保温3-6h,加入改性氧化铝、组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,热处理,冷却至室温,脱模,得到聚酰亚胺薄膜。
作为本发明的进一步方案:S1中纳米氧化铝、N,N-二甲基甲酰胺、偏苯三酸酐、二月桂酸二丁基锡的添加比为10g:100-200mL:1-5g:0.05-0.5g。
作为本发明的进一步方案:S2中八甲基环四硅氧烷、八苯基环四硅氧烷、1,3-双(3氨基丙基)四甲基二硅氧烷、四甲基铵硅烷醇的质量比为1-2:3-6:2-5:0.03-0.1。
作为本发明的进一步方案:S3中N,N′-二甲基乙酰胺、4,4′-二氨基二苯醚、均苯四甲酸二酐、改性氧化铝、组分一的质量比为10-25:1:1-2:0.15-0.35:0.1-0.5。
作为本发明的进一步方案:S4中热处理具体步骤为:置于真空干燥箱中阶梯程序升温:(80-100)℃×(1-3)h、(120-150)℃×(1-2)h、(200-240)℃×(1-2)h、(250-300)℃×(0.5-1)h。
作为本发明的进一步方案:聚酰亚胺薄膜层厚度为0.025-0.050mm。
作为本发明的进一步方案:云母纸层是定量为70-180g/cm2的非煅烧型白粉云母纸;云母纸的厚度为0.05-0.12mm。
作为本发明的进一步方案:无碱玻璃布层是定量为17-25g/cm2的电工无碱玻璃布;无碱玻璃布层厚度0.02-0.05mm。
作为本发明的进一步方案:所述第一胶粘剂层为胶粘剂涂覆在聚酰亚胺薄膜层一侧得到;第一胶粘剂层的质量占云母带总质量的5-10%;第二胶粘剂层为胶粘剂涂覆在无碱玻璃布层一侧得到;第二胶粘剂层的质量占云母带总质量的1-5%。
作为本发明的进一步方案:所述胶粘剂包括如下重量份的原料:40-50份有机硅改性环氧树脂、1-5份气相二氧化硅、5-10份己二酸、0.1-1份乙酰丙酮铬;3-15份溶剂;溶剂为甲苯、二甲苯、丁酮、丙酮、乙酸乙酯中的一种或多种以任意比混合得到。
作为本发明的进一步方案:所述有机硅改性环氧树脂的制备方法包括如下步骤:
C1:氮气氛围中,将80-100g八甲基环四硅氧烷、3-5g N-β-胺乙基-γ氨丙基甲基二硅氧烷加入反应瓶中,分散均匀,加入8-12g氢氧化钾、0.05-0.5g六甲基二硅氧烷,分散均匀,控制温度80-100℃,保温6-9h,得到氨基硅油;
C2:将100g的氨基硅油、4-8g的环氧树脂(ECC202)加入反应瓶中,控制温度90-110℃,保温0.5-1h,控制温度70-80℃,加入3-5g 4,4′-二氨基二苯甲烷(固化剂),搅拌均匀,得到有机硅改性环氧树脂。
一种自粘聚酰亚胺云母带的生产工艺,包括如下步骤:
A1:在聚酰亚胺薄膜层一侧涂覆第一胶粘剂,烘焙,制得具备第一胶粘剂层的复合层一;
A2:在无碱玻璃布层一侧涂覆第二胶粘剂,制得具备第二胶粘剂层的复合层二;
A3:复合层二通过第二胶粘剂层与云母纸层复合,烘焙,制得具备云母纸层(1)的复合层三;
A4:复合层一通过第一胶粘剂层与复合层三复合,所述第一胶粘剂层设置在聚酰亚胺薄膜层和云母纸层之间,得到云母带。
作为本发明的进一步方案:A4中复合具体内容为:90-120℃下烘烤5-10min。
本发明的有益效果:
(1)本申请首先利用偏苯三酸酐对纳米氧化铝进行改性,得到改性氧化铝;本申请制备的改性氧化铝表面具有丰富的羧基,在纳米粒子表面包裹一层有机物膜,形成较大的空间位阻,有效阻止纳米粒子团聚,改善纳米粒子在基体中的稳定性,提高与有机体的相容性。本申请将改性后的氧化铝添加在聚酰胺酸制备过程中,通过组分一将改性氧化铝与聚酰亚胺分子链进行交联,粒子表面包裹的有机物与聚酰亚胺分子链发生化学反应,产生化学键连接,增强膜中有机相和无机相之间的相互作用,有效提高聚酰亚胺的耐热性、力学性能和电学性能,并利用组分一的硅氧键Si-O键,赋予聚酰亚胺低的热膨胀系数和低吸水率的特性,在聚酰亚胺中形成互穿的网络结构,使聚酰亚胺的耐热性提高,热膨胀系数降低,改善聚合物的力学性能和韧性。
(2)本申请利用组分一将氧化铝和聚酰亚胺分子链交联,使聚酰亚胺分子链在局部放电时不易被破坏,局部放电后残留下的改性氧化铝聚集在固体介质表面并形成絮状结构,改性氧化铝在电场作用下具有自迁移特性,聚酰亚胺基体局部区域熔融或降解后,析出的纳米粒子在电场作用下迁移到此处以平衡电场,有效阻止带电粒子对有机物的撞击,从而抑制其对聚合物的进一步侵蚀、避免进一步介质击穿;析出的氧化铝与胶粘剂粘附性能好,有效提高云母带在使用过程中的绝缘稳定性。
(3)本申请将均苯四甲酸二酐和4,4′-二氨基二苯醚在非质子极性溶剂(N,N′-二甲基乙酰胺)中进行低温溶液聚合,获得聚酰胺酸溶剂,并利用聚酰胺酸溶剂进行热亚胺化,得到聚酰亚胺薄膜;在聚酰胺酸制备过程中,通过添加组分一和改性氧化铝;本申请通过反应将组分一接枝聚酰胺酸分子链将含醚、含硅等柔性基团引入到聚酰亚胺链段中,聚酰亚胺的刚性链段作用力减弱、分子链之间的作用力减弱,有效提高聚合物的韧性,提高聚酰亚胺的加工流动性;本申请利用氧化铝的表面和界面效应特性,提高材料的刚性和韧性;并利用改性氧化铝表面羧基基团,增加薄膜的亲水性能、水接触角降低,薄膜的粘附功能提高。解决纯聚酰亚胺薄膜因表面光滑以及低表面化学活性,与基材的界面粘结性能差的问题。本申请制备的聚酰亚胺薄膜复合云母带是一种以云母纸为基材,粘合聚酰亚胺薄膜、无碱玻璃布层组成的绝缘材料,具有优秀的耐热性能、力学性能以及电气性能,在耐高温电机领域应用广泛。
附图说明
下面结合附图对本发明作进一步的说明。
图1是本发明云母带结构示意图。
附图中,各标号所代表的部件列表如下:
1、云母纸层;2、聚酰亚胺薄膜层;3、无碱玻璃布层;4、第一胶粘剂层;5、第二胶粘剂层。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1 有机硅改性环氧树脂的制备方法包括如下步骤:
C1:氮气氛围中,将80g八甲基环四硅氧烷、3g N-β-胺乙基-γ氨丙基甲基二硅氧烷加入反应瓶中,分散均匀,加入10g氢氧化钾、0.2g六甲基二硅氧烷,分散均匀,控制温度90℃,保温6h,得到氨基硅油;
C2:将100g氨基硅油、4-8g环氧树脂(ECC202)加入反应瓶中,控制温度110℃,保温1h,控制温度70℃,加入5g 4,4′-二氨基二苯甲烷,搅拌均匀,得到有机硅改性环氧树脂。
实施例2 聚酰亚胺薄膜层2的制备方法包括如下步骤:
S1:氮气氛围中,将50g纳米氧化铝、1000mL N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入10g偏苯三酸酐,分散均匀,加入1g二月桂酸二丁基锡,控制温度110℃,搅拌条件下保温9h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将100g八甲基环四硅氧烷、400g八苯基环四硅氧烷、300g 1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度100℃,加入5g 四甲基铵硅烷醇,保温反应24h,控制温度160℃,保温1h,控制温度110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将1000g N,N′-二甲基乙酰胺、100g均苯四甲酸二酐加入反应釜B中,分散均匀,加入100g 4,4′-二氨基二苯醚,控制温度0℃,搅拌条件下保温3h,加入15g改性氧化铝、20g组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,置于真空干燥箱中阶梯程序升温:80℃×3h、120℃×1h、200℃×2h、300℃×1h,冷却至室温,脱模,得到厚度为0.025mm的聚酰亚胺薄膜。
实施例3 聚酰亚胺薄膜层2的制备方法包括如下步骤:
S1:氮气氛围中,将50g纳米氧化铝、1000mL N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入10g偏苯三酸酐,分散均匀,加入1g二月桂酸二丁基锡,控制温度110℃,搅拌条件下保温9h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将100g八甲基环四硅氧烷、400g八苯基环四硅氧烷、300g 1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度100℃,加入5g 四甲基铵硅烷醇,保温反应24h,控制温度160℃,保温1h,控制温度110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将1000g N,N′-二甲基乙酰胺、100g均苯四甲酸二酐加入反应釜B中,分散均匀,加入100g 4,4′-二氨基二苯醚,控制温度0℃,搅拌条件下保温3h,加入25g改性氧化铝、20g组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,置于真空干燥箱中阶梯程序升温:80℃×3h、120℃×1h、200℃×2h、300℃×1h,冷却至室温,脱模,得到厚度为0.025mm的聚酰亚胺薄膜。
实施例4 聚酰亚胺薄膜层2的制备方法包括如下步骤:
S1:氮气氛围中,将50g纳米氧化铝、1000mL N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入10g偏苯三酸酐,分散均匀,加入1g二月桂酸二丁基锡,控制温度110℃,搅拌条件下保温9h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将100g八甲基环四硅氧烷、400g八苯基环四硅氧烷、300g 1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度100℃,加入5g 四甲基铵硅烷醇,保温反应24h,控制温度160℃,保温1h,控制温度110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将1000g N,N′-二甲基乙酰胺、100g均苯四甲酸二酐加入反应釜B中,分散均匀,加入100g 4,4′-二氨基二苯醚,控制温度0℃,搅拌条件下保温3h,加入35g改性氧化铝、20g组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,置于真空干燥箱中阶梯程序升温:80℃×3h、120℃×1h、200℃×2h、300℃×1h,冷却至室温,脱模,得到厚度为0.025mm的聚酰亚胺薄膜。
实施例5 一种自粘聚酰亚胺云母带的生产工艺,包括如下步骤:
A1:按下述重量份的原料混合制备胶粘剂:40份实施例1制备的有机硅改性环氧树脂、3份气相二氧化硅、5份己二酸、0.5份乙酰丙酮铬;3-15份甲苯。
A2:在实施例2制备的聚酰亚胺薄膜层2一侧涂覆胶粘剂,烘焙,制得具备第一胶粘剂层4的复合层一,第一胶粘剂层的质量占云母带总质量的5%;
A3:在无碱玻璃布层3(无碱玻璃布层是定量为20.4g/cm2的电工无碱玻璃布;无碱玻璃布层厚度0.02mm)一侧涂覆胶粘剂,制得具备第二胶粘剂层5的复合层二,第二胶粘剂层的质量占云母带总质量的2%;
A4:复合层二通过第二胶粘剂层5与云母纸层1(云母纸层是定量为74.2g/cm2的非煅烧型白粉云母纸;云母纸的厚度为0.05mm)复合,烘焙,制得具备云母纸层1的复合层三;
A5:复合层一通过第一胶粘剂层4与复合层三复合并置于90-120℃下烘烤5-10min,第一胶粘剂层4设置在聚酰亚胺薄膜层2和云母纸层1之间,得到云母带。
实施例6 与实施例5相比,实施例6中仅仅将实施例5中使用的实施例2制备的聚酰亚胺薄膜替换成实施例3制备的聚酰亚胺薄膜,其余组分和步骤与实施例5完全一致。
实施例7 与实施例5相比,实施例7中仅仅将实施例5中使用的实施例2制备的聚酰亚胺薄膜替换成实施例4制备的聚酰亚胺薄膜,其余组分和步骤与实施例5完全一致。
对比例1 聚酰亚胺薄膜层2的制备方法包括如下步骤:
S1:氮气氛围中,将100g八甲基环四硅氧烷、400g八苯基环四硅氧烷、300g 1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度100℃,加入5g 四甲基铵硅烷醇,保温反应24h,控制温度160℃,保温1h,控制温度110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将1000g N,N′-二甲基乙酰胺、100g均苯四甲酸二酐加入反应釜B中,分散均匀,加入100g 4,4′-二氨基二苯醚,控制温度0℃,搅拌条件下保温3h,加入15g纳米氧化铝、20g组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,置于真空干燥箱中阶梯程序升温:80℃×3h、120℃×1h、200℃×2h、300℃×1h,冷却至室温,脱模,得到厚度为0.025mm的聚酰亚胺薄膜。
对比例2 聚酰亚胺薄膜层2的制备方法包括如下步骤:
S1:氮气氛围中,将50g纳米氧化铝、1000mL N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入10g偏苯三酸酐,分散均匀,加入1g二月桂酸二丁基锡,控制温度110℃,搅拌条件下保温9h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将1000g N,N′-二甲基乙酰胺、100g均苯四甲酸二酐加入反应釜B中,分散均匀,加入100g 4,4′-二氨基二苯醚,控制温度0℃,搅拌条件下保温3h,加入15g改性氧化铝,搅拌条件下保温3-6h,得到混合液;
S3:将混合液在洁净玻璃板上延流成膜,置于真空干燥箱中阶梯程序升温:80℃×3h、120℃×1h、200℃×2h、300℃×1h,冷却至室温,脱模,得到厚度为0.025mm的聚酰亚胺薄膜。
对比例3 与实施例5相比,对比例3中仅仅将实施例5中使用的实施例2制备的聚酰亚胺薄膜替换成对比例1制备的聚酰亚胺薄膜,其余组分和步骤与实施例5完全一致。
对比例4 与实施例5相比,对比例4中仅仅将实施例5中使用的实施例2制备的聚酰亚胺薄膜替换成对比例2制备的聚酰亚胺薄膜,其余组分和步骤与实施例5完全一致。
性能检测
(1)力学性能:根据GB/T 13542.2-2009《电气绝缘用薄膜》中第11章的标准进行检测,采用日本岛津公司的AGS-J型电子万能试验机,对实施例2-4、对比例1-2聚酰亚胺薄膜的拉伸强度及断裂伸长率进行测试,拉伸速度为50mm/min,夹具间距离为100mm;检测结果见表1;
(2)耐电晕性能:根据T/CEEIA438-2020《电气绝缘用耐电晕聚酰亚胺薄膜技术要求》进行检测,采用桂林电器科学研究所的HP-3kV高频脉冲电压测试仪,对实施例2-4、对比例1-2聚酰亚胺薄膜耐电晕性能进行测试,测试条件:脉冲波形及极性为双极性对称方波,脉冲频率为20kHz,脉冲上升沿时间(负载)为100ns,脉冲占空比为50%,脉冲电压(U)为2.0kV,温度为室温;检测结果见表1;
表1:实施例2-4、对比例1-2聚酰亚胺薄膜性能检测数据统计表
(3)抗老化性能:根据GB/T 11026.1-2003《电气绝缘材料耐热性第1部分:老化程序和试验结果的评定》进行检测,选取中温点280℃,对薄膜进行200h、600h、1000h热老化试验,并检测各老化时段与初始的拉伸强度、电气强度的数值留存率,检测结果见表2;
表2:实施例2-4、对比例1-2抗老化性能检测数据统计表
(4)击穿电压:根据GB/T 1408.1-2006《绝缘材料电气强度试验方法 第1部分:工频下试验》进行测试,对实施例5-7、对比例3-4制备的云母带进行检测,将长度为0.25m的定宽云母带放置在橡胶垫片上,采用直径6mm的电极,升压速度为500V/s,直至云母带击穿,记录此时的击穿电压值。测量前需要校零,结果取10个测试值的中值,检测结果见表3;
表3:云母带性能检测数据统计表
由表1-3可知,本申请制备具有耐电晕、粘结性能强以及耐老化效果好的特点,本申请制备的聚酰亚胺薄膜以及无碱玻璃布层作为增强层、与云母纸层复合制备云母带,得到的云母带应用在变频电机中具有优良的绝缘稳定性。
以上对本发明的一个实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。
Claims (10)
1.一种自粘聚酰亚胺云母带,其特征在于,所述云母带包括云母纸层(1),所述云母纸层(1)一侧设置聚酰亚胺薄膜层(2)、另一侧设置有无碱玻璃布层(3),所述云母纸层(1)与聚酰亚胺薄膜层(2)通过第一胶粘剂层(4)复合,所述云母纸层(1)与无碱玻璃布层(3)通过第二胶粘剂层(5)复合;
所述聚酰亚胺薄膜层(2)的制备方法包括如下步骤:
S1:氮气氛围中,将纳米氧化铝、N,N-二甲基甲酰胺加入反应釜A中,分散均匀,加入偏苯三酸酐,分散均匀,加入二月桂酸二丁基锡,控制温度110-120℃,搅拌条件下保温9-12h,洗涤、分离、干燥,得到改性氧化铝;
S2:氮气氛围中,将八甲基环四硅氧烷、八苯基环四硅氧烷、1,3-双(3氨基丙基)四甲基二硅氧烷加入反应瓶中,控制温度90-100℃,加入四甲基铵硅烷醇,保温反应24-36h,控制温度160-165℃,保温0.5-1h,控制温度100-110℃下真空除去低沸物,得到组分一;
S3:氮气氛围中,将N,N′-二甲基乙酰胺、均苯四甲酸二酐加入反应釜B中,分散均匀,加入4,4′-二氨基二苯醚,控制温度0-5℃,搅拌条件下保温3-6h,加入改性氧化铝、组分一,搅拌条件下保温3-6h,得到混合液;
S4:将混合液在洁净玻璃板上延流成膜,热处理,冷却至室温,脱模,得到聚酰亚胺薄膜。
2.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,S1中纳米氧化铝、N,N-二甲基甲酰胺、偏苯三酸酐、二月桂酸二丁基锡的添加比为10g:100-200mL:1-5g:0.05-0.5g。
3.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,S2中八甲基环四硅氧烷、八苯基环四硅氧烷、1,3-双(3氨基丙基)四甲基二硅氧烷、四甲基铵硅烷醇的质量比为1-2:3-6:2-5:0.03-0.1。
4.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,S3中N,N′-二甲基乙酰胺、4,4′-二氨基二苯醚、均苯四甲酸二酐、改性氧化铝、组分一的质量比为10-25:1:1-2:0.15-0.35:0.1-0.5。
5.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,聚酰亚胺薄膜层厚度为0.025-0.050mm。
6.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,云母纸层是定量为70-180g/cm2的非煅烧型白粉云母纸;云母纸的厚度为0.05-0.12mm。
7.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,无碱玻璃布层是定量为17-25g/cm2的电工无碱玻璃布;无碱玻璃布层厚度0.02-0.05mm。
8.根据权利要求1所述的一种自粘聚酰亚胺云母带,其特征在于,所述第一胶粘剂层为胶粘剂涂覆在聚酰亚胺薄膜层一侧得到;第一胶粘剂层的质量占云母带总质量的5-10%;第二胶粘剂层为胶粘剂涂覆在无碱玻璃布层一侧得到;第二胶粘剂层的质量占云母带总质量的1-5%。
9.根据权利要求8所述的一种自粘聚酰亚胺云母带,其特征在于,所述胶粘剂包括如下重量份的原料:40-50份有机硅改性环氧树脂、1-5份气相二氧化硅、5-10份己二酸、0.1-1份乙酰丙酮铬;3-15份溶剂;溶剂为甲苯、二甲苯、丁酮、丙酮、乙酸乙酯中的一种或多种以任意比混合得到。
10.一种自粘聚酰亚胺云母带的生产工艺,其特征在于,包括如下步骤:
A1:在聚酰亚胺薄膜层(2)一侧涂覆第一胶粘剂,烘焙,制得具备第一胶粘剂层(4)的复合层一;
A2:在无碱玻璃布层(3)一侧涂覆第二胶粘剂,制得具备第二胶粘剂层(5)的复合层二;
A3:复合层二通过第二胶粘剂层(5)与云母纸层(1)复合,烘焙,制得具备云母纸层(1)的复合层三;
A4:复合层一通过第一胶粘剂层(4)与复合层三复合,所述第一胶粘剂层(4)设置在聚酰亚胺薄膜层(2)和云母纸层(1)之间,得到云母带。
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