CN114836003A - 一种汽车用酚醛树脂棉布层压板及其制备方法 - Google Patents
一种汽车用酚醛树脂棉布层压板及其制备方法 Download PDFInfo
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 85
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 85
- 229920000742 Cotton Polymers 0.000 title claims abstract description 73
- 239000004744 fabric Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003292 glue Substances 0.000 claims abstract description 48
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 31
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- 239000000463 material Substances 0.000 claims abstract description 16
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims abstract description 15
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 16
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- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
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- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明公开了一种汽车用酚醛树脂棉布层压板及其制备方法,所述层压板,包括多层在改性胶液进行处理的增强材料,所述增强材料包括无纺布;所述改性胶液,包括以下质量份的原料:复合酚醛树脂溶液100‑120份、邻苯二甲酸二丁酯1‑3份、乙酰柠檬酸三丁酯0.2‑0.5份、偶联剂0.1‑0.5份、分散剂2‑4份。本发明通过改性胶液的制备,将无纺布浸渍后,经过压制成型得到的层压板,具有较低的吸水率以及优异的机械性能。
Description
技术领域
本发明属于层压板领域,具体涉及一种汽车用酚醛树脂棉布层压板及其制备方法。
背景技术
层压板是由两层或多层浸有树脂的纤维或织物经叠合、热压结合成的整体。层压板的性能取决于基材和粘合剂以及成型工艺。按其组成、特性和耐热性,层压板可分为以下两种。
1、有机基材层压板:以木浆绝缘纸、棉纤维纸、棉布等为增强材料。长期使用温度可达120℃,还发展了合成纤维制品为增强材料。
2、无机基材层压板:以无机玻璃纤维布、无碱玻璃纤维毡等为增强材料。长期使用温度为130~180℃,甚至可达更高温度,随粘合树脂而异。
当前的酚醛棉布层压板是由棉布浸以酚醛树脂经烘干热压而成,具有高的机械性能,适用于机械、电机、电器设备中作绝缘结构零部件,并可在变压器油中使用。一般的酚醛棉布层压板,由于棉布和普通酚醛树脂的耐热性差,致使其产品使用寿命缩短。
而棉布为棉纱织成的布,是各类棉纺织品的总称,它多用来制作时装、休闲装、内衣和衬衫;当前存在着较多的旧棉布,常常将其丢弃,造成了资源的浪费,因此有必要提出一种利用旧棉布来生产汽车用酚醛树脂棉布层压板及其制备方法。
发明内容
本发明为解决现有技术的上述问题,本发明采用以下技术方案:
一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料,所述增强材料包括将旧棉布处理而得的无纺布;
所述改性胶液,包括以下质量份的原料:
复合酚醛树脂溶液100-120份、邻苯二甲酸二丁酯1-3份、乙酰柠檬酸三丁酯0.2-0.5份、偶联剂0.1-0.5份、分散剂2-4份;
所述偶联剂为铝酸酯偶联剂,可以改善制品的物理性能,如提高冲击强度和热变形温度方面;并且具有成本较低、色浅无毒、使用方便等特点。
进一步的,所述分散剂为脂肪酸聚乙二醇酯;通过脂肪酸聚乙二醇酯的加入,可以提升复合酚醛树脂溶液中各个组分的分散性,保持改性胶液的均一性。
进一步的,所述复合酚醛树脂溶液,包括以下重量份的原料:
酚醛树脂25-30份、环氧树脂5-10份、SBS树脂6-8份、溶剂63-70份、稳定剂1-2份。
进一步的,所述酚醛树脂为线型双酚A酚醛树脂;所述酚醛树脂能够很好地和环氧树脂共融,且环氧树脂中的环氧基可以和酚醛树脂中的酚羟基和羟甲基进行反应,可以固化酚醛树脂,进而提升酚醛树脂的高温稳定性以及耐热性、尺寸稳定性,而且采用的线型双酚A酚醛树脂和环氧树脂共融性较好,可改善茶色斑点以及变色的问题;
在本发明中,环氧树脂可选用双酚F型环氧树脂,其具有是黏度小,对棉纤维的浸渍性好的特点。
在本发明中,SBS树脂,具有优良的拉伸强度、弹性和电性能.永久变形小,屈挠和回弹性好,表面摩擦大,耐臭氧、氧和紫外线照射性能与丁苯橡胶类似,透气性优异;所述SBS树脂作为增容树脂以及增韧树脂,可以提升体系的粘接能力,进而提升浸渍效果,且提高环氧树脂在酚醛树脂中的共融能力。具体的SBS树脂选用线型SBS树脂。
进一步的,所述溶剂包括甲醇、乙酸乙酯中的任一种或两种;通过溶剂的加入,溶融酚醛树脂、环氧树脂、SBS树脂,方便增强材料的浸渍;
进一步的,所述稳定剂为聚酯纤维,平均长度为5-6mm,,通过稳定剂的加入,稳定复合酚醛树脂溶液,方便后续改性胶液的上胶到增强材料以及改性胶液固化的进行。而且稳定剂,可以起到减慢反应、保持化学平衡、降低表面张力、防止光、热分解或氧化分解等作用。
更进一步的,所述旧棉布为废涤棉混纺纺织品;
在本发明中,通过加入邻苯二甲酸二丁酯,可以插入聚合物分子链之间,削弱了聚合物分子链间的作用力,结果增大了聚合物分子链的移动性,降低了聚合物分子链的结晶度,从而使聚合物的塑性增加,而且与树脂具有良好的相容性,可以提高树脂的耐久性、耐寒性。
在本发明中,通过加入乙酰柠檬酸三丁酯,可以提升邻苯二甲酸二丁酯在胶液中的溶解性,方便浸渍的进行;因为与多种纤维素、乙烯基树脂、氯化橡胶等相容,与醋酸纤维素、醋酸丁酯纤维素部分相容。
一种汽车用酚醛树脂棉布层压板的制备方法,包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行充分混合后,升温至60-65℃,加入SBS树脂,进行搅拌;加入环氧树脂,进行搅拌,再加入稳定剂,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;将复合酚醛树脂溶液和分散剂进行充分混合后,加入偶联剂,搅拌,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯,进行搅拌,静置,得到改性胶液;待用;
S3、旧棉布处理
将旧棉布洗净晾干后,经过醇解得到的涤纶和棉纤维经涤棉过滤器,得到棉纤维;将棉纤维经过铺网整理,再经过水刺处理得到无纺布;
S4.浸渍处理
在步骤S3制备得到的无纺布,使用步骤S2制备得到的改性胶液,进行上胶,浸渍结束后进行干燥处理,得到半固化片;
S5.压制成型
将多层半固化片叠在一起,进行压制成型,得到所述层压板。
进一步的,所述水刺处理过程为,将棉纤维网在水刺压力为50-60*105pa下固定。
与现有技术相比,本发明具有以下有益效果:
1、通过改性胶液的制备,将无纺布浸渍后,经过压制成型,得到的层压板,具有较低的吸水率以及优异的机械性能。
2、通过将废涤棉混纺纺织品制备得到无纺布,再结合改性胶液浸渍及压制成型,得到的层压板,明显提高了耐热度。
3、本发明制备得到的层压板,未检出甲醛的释放,且在高温高湿的环境下可以长期使用。
具体实施方式
下面进一步描述本发明的技术方案,但要求保护的范围并不局限于所述。
实施例1
本发明所述的,将旧棉布处理而得的无纺布;该无纺布具体制备过程为:
称取废涤棉混纺纺织品120Kg/h,进入螺杆熔融,同时往螺杆加入乙二醇600Kg/h,在常压、温度为200℃下醇解10min,经碎布熔融机进行醇解熔融后,再经涤棉过滤系统处理(经涤棉过滤器处理),回收棉纤维;将棉纤维蒸干后,使用梳理机将开松后的棉纤维理顺,将梳理而成的棉纤维重叠铺网,将棉纤维制成棉纤维网;将棉纤维网进行水刺工艺处理,使棉纤维缠结成无纺布;具体水刺工艺处理为:棉纤维网在水刺压力为50-60*105pa下固定。上述步骤可得到可得到厚度为0.4-0.5mm的无纺布。无纺布的撕裂强度为20-21N。
实施例2
一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料,
所述改性胶液,包括以下质量份的原料:
邻苯二甲酸二丁酯1份、乙酰柠檬酸三丁酯0.2份、铝酸酯偶联剂0.1份、脂肪酸聚乙二醇酯2份;线型双酚A酚醛树脂25份、双酚F型环氧树脂5份、线型SBS树脂6份;甲醇33份、乙酸乙酯30份;稳定剂1份,具体为聚酯纤维,平均长度为5-6mm;
上述汽车用酚醛树脂棉布层压板的制备方法,包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行搅拌,搅拌速度100r/mim,混合1h后,升温至60℃,加入SBS树脂,搅拌速度80r/mim,混合1h;加入环氧树脂,进行搅拌,搅拌速度80r/mim,混合1h,再加入稳定剂,搅拌速度80r/mim,混合1h,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;在35℃下,将复合酚醛树脂溶液和分散剂进行搅拌,搅拌速度50r/mim,混合10min后,加入偶联剂;搅拌,搅拌速度50r/mim,混合5min,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯;搅拌,搅拌速度50r/mim,混合5min,降至室温,得到改性胶液;待用;
S3、旧棉布处理
按照实施例1进行
S4.浸渍处理
在步骤S3制备得到的无纺布,在卧式浸胶槽浸渍改性胶液进行上胶,无纺布浸渍速度为3m/min;浸渍结束后,在130℃下干燥5min,得到半固片;得到半固片;半固片控制含胶量50-51%;
S5.压制成型
将多层步骤S4得到的半固化片叠加后,在100℃下预热15min升温至150℃,在80Kg/cm2下压制2h,降温冷却到室温,得到所述层压板。
实施例3
一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料;
所述改性胶液,包括以下质量份的原料:
邻苯二甲酸二丁酯2份、乙酰柠檬酸三丁酯0.3份、铝酸酯偶联剂0.3份、脂肪酸聚乙二醇酯3份;线型双酚A酚醛树脂28份、双酚F型环氧树脂7份、线型SBS树脂7份;甲醇20份、乙酸乙酯46份;稳定剂1.5份,具体为聚酯纤维,平均长度为5-6mm;
上述汽车用酚醛树脂棉布层压板的制备方法,包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行搅拌,搅拌速度130r/mim,混合1h后,升温至63℃,加入SBS树脂,搅拌速度90r/mim,混合1h;加入环氧树脂,进行搅拌,搅拌速度90r/mim,混合1h,再加入稳定剂,搅拌速度90r/mim,混合1h,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;在38℃下,将复合酚醛树脂溶液和分散剂进行搅拌,搅拌速度55r/mim,混合10min后,加入偶联剂;搅拌,搅拌速度55r/mim,混合5min,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯;搅拌,搅拌速度55r/mim,混合5min,降至室温,得到改性胶液;待用;
S3、旧棉布处理
按照实施例1进行
S4.浸渍处理
在步骤S3制备得到的无纺布,在卧式浸胶槽浸渍改性胶液进行上胶,无纺布浸渍速度为3.5m/min;浸渍结束后,在133℃下干燥7min,得到半固片;半固片控制含胶量51-53%;
S5.压制成型
将多层步骤S4得到的半固化片叠加后,在105℃下预热18min升温至155℃,在85Kg/cm2下压制2.3h,降温冷却到室温,得到所述层压板。
实施例4
一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料,
所述改性胶液,包括以下质量份的原料:
邻苯二甲酸二丁酯3份、乙酰柠檬酸三丁酯0.5份、铝酸酯偶联剂0.5份、脂肪酸聚乙二醇酯4份;线型双酚A酚醛树脂30份、双酚F型环氧树脂10份、线型SBS树脂8份;甲醇35份、乙酸乙酯35份;稳定剂2份,具体为聚酯纤维,平均长度为6mm;
上述汽车用酚醛树脂棉布层压板的制备方法,包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行搅拌,搅拌速度150r/mim,混合1h后,升温至65℃,加入SBS树脂,搅拌速度100r/mim,混合1h;加入环氧树脂,进行搅拌,搅拌速度100r/mim,混合1h,再加入稳定剂,搅拌速度100r/mim,混合1h,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;在40℃下,将复合酚醛树脂溶液和分散剂进行搅拌,搅拌速度60r/mim,混合10min后,加入偶联剂;搅拌,搅拌速度60r/mim,混合5min,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯;搅拌,搅拌速度60r/mim,混合5min,降至室温,得到改性胶液;待用;
S3、旧棉布处理
按照实施例1进行
S4.浸渍处理
在步骤S3制备得到的无纺布,在卧式浸胶槽浸渍改性胶液进行上胶,无纺布浸渍速度为4m/min;浸渍结束后,在135℃下干燥8min,得到半固片;得到半固片;半固片控制含胶量55%;
S5.压制成型
将多层步骤S4得到的半固化片叠加后,在110℃下预热20min升温至160℃,在90Kg/cm2下压制2.5h,降温冷却到室温,得到所述层压板。
实施例5
一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料,
所述改性胶液,包括以下质量份的原料:
邻苯二甲酸二丁酯1份、乙酰柠檬酸三丁酯0.4份、铝酸酯偶联剂0.5份、脂肪酸聚乙二醇酯2份;线型双酚A酚醛树脂30份、双酚F型环氧树脂5份、线型SBS树脂8份;甲醇30份、乙酸乙酯40份;稳定剂1份,具体为聚酯纤维,平均长度为5-6mm;
上述汽车用酚醛树脂棉布层压板的制备方法,包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行搅拌,搅拌速度100r/mim,混合1h后,升温至65℃,加入SBS树脂,搅拌速度80r/mim,混合1h;加入环氧树脂,进行搅拌,搅拌速度100r/mim,混合1h,再加入稳定剂,搅拌速度80r/mim,混合1h,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;在35℃下,将复合酚醛树脂溶液和分散剂进行搅拌,搅拌速度60r/mim,混合10min后,加入偶联剂;搅拌,搅拌速度50r/mim,混合5min,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯;搅拌,搅拌速度60r/mim,混合5min,降至室温,得到改性胶液;待用;
S3、旧棉布处理
按照实施例1进行
S4.浸渍处理
在步骤S3制备得到的无纺布,在卧式浸胶槽浸渍改性胶液进行上胶,无纺布浸渍速度为4m/min;浸渍结束后,在135℃下干燥5min,得到半固片;得到半固片;半固片控制含胶量52-53%;
S5.压制成型
将多层步骤S4得到的半固化片叠加后,在100℃下预热15min升温至160℃,在90Kg/cm2下压制2h,降温冷却到室温,得到所述层压板。
对比例1
将步骤S3中的无纺布,变为干净的还未使用过的棉布(大小厚度和该无纺布一致);其余条件和实施例2一致。
对比例2
所述改性胶液,包括以下质量份的原料:
邻苯二甲酸二丁酯1份、乙酰柠檬酸三丁酯0.2份、铝酸酯偶联剂0.1份、脂肪酸聚乙二醇酯2份;线型双酚A酚醛树脂25份;甲醇33份、乙酸乙酯30份;稳定剂1份,具体为聚酯纤维,平均长度为5-6mm;其余条件和实施例2一致;
将实施例2-实施例4,以及对比例1-2制备得到的层压板,进行性能检测,相关结果如下表1所示:
表1
从上述结果可以看出,实施例2-实施例5制备得到的层压板,具有较低的吸水率,吸水率仅仅为0.02-0.06%;具有较高的机械性能,其中拉伸强度达到138-146MPa,弯曲强度126-134MPa,而耐热度在达到了183℃以上,可以应用在建筑、汽车等领域。
对比例1的起始为干净的棉布,棉布上一般还附有聚酯,有一定程度的影响和改性胶液和棉布的结合,造成吸水率略高;
对比例2,而对比例2,将无纺布直接和酚醛树脂结合,附着力略差,弯曲强度和拉伸强度也较差,同时由于酚醛树脂未经过改性偶联,将释放出甲醛,影响使用。
将上述实施例2、对比例1-2制备得到的层压板,在温度70℃+湿度65±5%下,作用1300h,测试吸湿后的性能,相关结果如下表2所示:
表2
因此可以看出,在经过高温高湿的作用下,实施例2的吸水率,基本上没什么发生变化,且拉伸强度达到137MPa,弯曲强度124MPa,拉伸强度和弯曲强度略微降低,说明了实施例2的层压板,胶液和无纺布结合牢靠,空隙小,可以保持较低的吸水率,因此能够保持较高的拉伸强度和弯曲强度。而对比例1的起始为干净的棉布,棉布上一般还附有聚酯,在长时间的高温高湿作用下,聚酯会吸水,造成膨胀,因此对比例1的吸湿率上升,进而造成了拉伸强度和弯曲强度的下降;而对比例2,将无纺布直接和酚醛树脂结合,附着力较差,在长时间的高温高湿作用下,有部分树脂脱离,使得对比例1的吸湿率明显上升,进而造成了拉伸强度和弯曲强度的大幅下降;
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的技术人员来说,在不脱离本发明构思的前提下,还可以做出若干等同替代或明显变型,而且性能或用途相同,都应当视为属于本发明。
Claims (10)
1.一种汽车用酚醛树脂棉布层压板,包括多层在改性胶液进行处理的增强材料,其特征在于:
所述增强材料包括无纺布;
所述改性胶液,包括以下质量份的原料:
复合酚醛树脂溶液100-120份、邻苯二甲酸二丁酯1-3份、乙酰柠檬酸三丁酯0.2-0.5份、偶联剂0.1-0.5份、分散剂2-4份。
2.根据权利要求1所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述偶联剂为铝酸酯偶联剂。
3.根据权利要求1所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述分散剂为脂肪酸聚乙二醇酯。
4.根据权利要求1所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述复合酚醛树脂溶液,包括以下重量份的原料:
酚醛树脂25-30份、环氧树脂5-10份、SBS树脂6-8份、溶剂63-70份、稳定剂1-2份。
5.根据权利要求4所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述酚醛树脂为线型双酚A酚醛树脂。
6.根据权利要求4所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述溶剂包括甲醇、乙酸乙酯中的任一种或两种。
7.根据权利要求4所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述稳定剂为聚酯纤维,平均长度为5-6mm。
8.根据权利要求1所述的一种汽车用酚醛树脂棉布层压板,其特征在于:所述无纺布为将废涤棉混纺纺织品处理成的布。
9.一种根据权利要求1-8任一项所述的汽车用酚醛树脂棉布层压板的制备方法,其特征在于:包括以下步骤:
S1.复合酚醛树脂溶液的制备
按照复合酚醛树脂溶液原料的重量份进行备料;将酚醛树脂和溶剂进行充分混合后,升温至60-65℃,加入SBS树脂,进行搅拌;加入环氧树脂,进行搅拌,再加入稳定剂,得到复合酚醛树脂溶液;待用;
S2.改性胶液的制备
按照改性胶液原料的重量份进行备料;将复合酚醛树脂溶液和分散剂进行充分混合后,加入偶联剂,搅拌,再加入邻苯二甲酸二丁酯、乙酰柠檬酸三丁酯进行搅拌,静置,得到改性胶液;待用;
S3、旧棉布处理
将旧棉布洗净晾干后,经过醇解得到的涤纶和棉纤维经涤棉过滤器,得到棉纤维;将棉纤维经过铺网整理,再经过水刺处理得到无纺布;
S4.浸渍处理
在步骤S3制备得到的无纺布,使用步骤S2制备得到的改性胶液,进行上胶,浸渍结束后进行干燥处理,得到半固化片;
S5.压制成型
将多层步骤S4得到的半固化片,进行压制成型,得到所述层压板。
10.根据权利要求9所述的一种汽车用酚醛树脂棉布层压板的制备方法,其特征在于:所述水刺处理过程为,棉纤维网在水刺压力为50-60*105pa下固定。
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