CN116638831A - 一种单体电芯间的高效隔热阻燃材料 - Google Patents
一种单体电芯间的高效隔热阻燃材料 Download PDFInfo
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- CN116638831A CN116638831A CN202310642827.1A CN202310642827A CN116638831A CN 116638831 A CN116638831 A CN 116638831A CN 202310642827 A CN202310642827 A CN 202310642827A CN 116638831 A CN116638831 A CN 116638831A
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- China
- Prior art keywords
- glass beads
- hollow glass
- modified
- retardant material
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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Abstract
本发明属于动力电池技术领域,公开了一种单体电芯间的高效隔热阻燃材料,包括芯层,所述芯层包是由二氧化硅气凝胶和空心陶瓷纤维复合的隔热纤维毡,所述芯层两侧包覆缓冲层,所述缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性的发泡聚氨酯,所述改性石墨烯为石墨烯经氧化还原后负载纳米氧化锌得到,所述改性空心玻璃微珠为玻璃微珠表面包覆纳米二氧化钛薄膜后接枝二苯基甲烷二异氰酸酯得到,本发明芯层通过空心陶瓷纤维对SO2气凝胶增强,提高了气凝胶纤维毡的隔热性能,缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性,料热稳定性和隔热性均得到提高。
Description
技术领域
本发明属于动力电池技术领域,具体涉及一种单体电芯间的高效隔热阻燃材料。
背景技术
国家大力发展新能源,电动汽车逐步进入市场,以后甚至替代燃油车成为未来交通工具的主流。众所周知的是电动车的续航里程和充电便利性是前期问题,但未来更为关键的是电池安全性。随着电动车续航里程增大需求,要求电池能量密度越来越高,随着电池能量密度逐渐增大,电池循环膨胀率逐步增大,由此引来的是电池自身安全性逐步下降,组成模组后,电芯之间膨胀力增大,电池发生热失控的概率增大。
为降低电池之间发生热失控的风险,电池之间通常安装隔热垫,通常希望一个电芯发生热失控急剧温升甚至着火时,不引起隔壁电芯连锁失控。因此,一方面,要求隔热垫具有较低的导热系数,同时满足阻燃要求(通常UL94-V0防火等级);另一方面,要求隔热垫具有缓冲功能,因为电芯在充放电循环工作时膨胀与收缩,这里电池膨胀与收缩简称“呼吸”,为保证高能量密度电池可以长寿命工作,做好加载在电芯两侧的力不能过大,以防压坏电芯内部结构,所以该隔热垫应具有缓冲回弹功能。
目前较为常用隔热材料主要有泡沫金属隔热材料、多孔有机隔热材料、有机纤维毡隔热材料、无机纤维毡隔热材料、多孔无机隔热材料等。这些隔热材料都有各自的优点和缺点,分别应用于不同的场合。例如:软木等天然多孔有机隔热材料价格便宜,方便获取,但隔热效果较差,一般用于温度较低的隔热场所。聚氨酯泡沫和酚醛泡沫材料等多孔有机隔热材料的导热系数较小,隔热效果好,但是聚氨酯泡沫的耐高温性能差,一般用于常温保温隔热;酚醛泡沫的烧蚀残留率高,纤维类隔热材料虽然具有隔热效果好、热稳定性好、质量轻、比热大及承受载荷大等优点,但是其气体阻隔性和柔性较差,难以制备出形状复杂的隔热材料,且加工工艺复杂。二氧化硅气凝胶是一种轻质高效的新型隔热材料,具有低密度、高孔隙率、低导热系数等特殊性能,但是其脆性大、强度低,且当温度较高时,气凝胶会失去其多孔结构而导致隔热性下降。
因此,亟需开发一种新型的隔热阻燃材料以解决电池电芯间的隔热问题。
发明内容
为解决上述背景技术中提到的不足,本发明的目的在于提供一种单体电芯间的高效隔热阻燃材料,芯层由二氧化硅气凝胶和空心陶瓷纤维复合的隔热纤维毡,通过空心陶瓷纤维增强,提高了气凝胶纤维毡的隔热性能,缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性的发泡聚氨酯,发泡聚氨酯材料热稳定性和隔热性均得到提高,同时发泡聚氨酯具有缓冲功能,对电芯在充放电循环工作时膨胀与收缩进行缓冲。
本发明的目的可以通过以下技术方案实现:
一种单体电芯间的高效隔热阻燃材料,其特征在于,包括芯层,所述芯层是由二氧化硅气凝胶和空心陶瓷纤维复合的隔热纤维毡,所述芯层两侧包覆缓冲层,所述缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性的发泡聚氨酯,所述改性石墨烯为石墨烯经氧化还原后负载纳米氧化锌得到,所述改性空心玻璃微珠为玻璃微珠表面包覆纳米二氧化钛薄膜后接枝二苯基甲烷二异氰酸酯得到;
所述缓冲层包括以下重量份原料:聚醚多元醇4110 80~120份、石油醚3~5份、丙三醇1~3份、二月桂酸二丁基锡0.01~0.2份、二甲基环己胺0.1~0.5份、二苯基甲烷二异氰酸酯100~110份、改性石墨烯5~10份、改性空心玻璃微珠10~15分、聚磷酸铵1~3份、季戊四醇0.5~1.5份。
进一步优选地,所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水加入容器中混合搅拌3~5min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1~2h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入空心陶瓷纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化12~24h;
(4)将老化后的复合材料按体积比1:2~4置于正己烷中进行溶剂交换12~24h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡12~24h,进行凝胶的表面基团改性;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后80~120℃干燥6~8h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
进一步优选地,所述步骤(1)中正硅酸乙酯、无水乙醇和去离子水按摩尔比为1:7:3。
进一步优选地,所述步骤(5)中三甲基氯硅烷和正己烷的体积比为1:8~10。
进一步优选地,所述空心陶瓷纤维的制备方法包括以下步骤:
先将木棉纤维浸入氯化铝及氯化镐的乙醇溶液中,充分浸渍后取出挤干,并在60~80℃下干燥;再将干燥后的木棉纤维以2~4℃/min的升温速率加热到800~1200℃,保温1~3h,随炉冷却后即制得空心陶瓷纤维。
进一步优选地,所述氯化铝及氯化镐的乙醇溶液中氯化铝及氯化镐的摩尔比为3~5:1。
进一步优选地,所述缓冲层的制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合5~10min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10~30s;最后,将均匀混合的原料倒入模具合膜后置于40~45℃的烘箱中发泡1~2h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
进一步优选地,所述改性石墨烯的制备方法包括以下步骤:
A、先将石墨加入浓H2SO4中并加热至80~90℃,使其与H2SO4发生反应,然后加入HNO3和KMnO4,进一步氧化石墨,形成氧化石墨烯,最后用水洗涤和离心分离,得到氧化石墨烯备用;
B、将氧化石墨烯加入水中超声分散得到氧化石墨烯分散液,然后将0.05~0.1mol/L的Zn(NO3)2溶液逐滴加入氧化石墨烯分散液中搅拌1~3h,最后用20%氨水调节pH值到10~11;
C、向混合液中加入NaBH4,密封后放入微波反应器内140~160℃反应8~10min,冷却过滤,用去离子水洗涤3~5次,70~80℃烘干得到改性石墨烯。
进一步优选地,所述改性空心玻璃微珠的制备方法包括以下步骤:
S1、将空心玻璃微珠加入80~90℃饱和Ca(OH)2溶液中浸泡处理8~10h,然后用去离子水洗涤干燥,得到表面粗糙化的空心玻璃微珠;
S2、将步骤S1处理后的空心玻璃微珠加入3~5wt%十二烷基苯磺酸钠水溶液中浸泡30~90min,烘干干燥得到表面活性剂处理的空心玻璃微珠;
S3、将步骤S2处理后的空心玻璃微珠加入蒸馏水中搅拌均匀得到悬浊液,60~80℃下均匀滴加10~15wt%的Ti(SO4)2溶液,同时用20%氨水调节pH至恒定,反应结束后静置冷却抽滤,蒸馏水洗涤2~3次后烘干煅烧,得到纳米TiO2包覆的空心玻璃微珠;
S4、将步骤S3得到的纳米TiO2包覆的空心玻璃微珠粉末加入到浓度为0.3mol/L的NaOH溶液中,70~80℃油浴锅中回流搅拌1~3h进行羟基化处理,然后减压抽滤同时用蒸馏水清洗玻璃微珠至其pH显中性,80~100℃真空干燥8~12h;
S5、将羟基化处理后的纳米TiO2包覆的空心玻璃微珠加入30%乙醇溶液中,然后向溶液中加入硅烷偶联剂KH550,70~80℃油浴锅中回流搅拌2~4h,用无水乙醇溶液进行反复洗涤、减压抽滤,80~100℃真空干燥8~12h;
S6、将步骤S5处理后的纳米TiO2包覆的空心玻璃微珠加入N,N-二甲基甲酰胺中,再加入的二苯基甲烷二异氰酸酯,70~80℃油浴锅中回流搅拌1~3h,最后用N,N-二甲基甲酰胺反复洗涤、减压抽滤,80~100℃真空干燥8~12h,得到所述改性空心玻璃微珠。
进一步优选地,所述空心玻璃微珠堆粒径为70~100μm,积密度为0.15~0.3g/cm3。
本发明的有益效果:
本发明
本发明通过石墨烯经氧化还原后负载纳米氧化锌得到的改性石墨烯,在燃烧过程中ZnO与APP反应,在APP之间形成桥键,少量的桥键可以增加APP的稳定性,降低热解过程中磷的挥发,在高温下ZnO还能促使APP脱氢、氧化和磷酸酯化,并形成不饱和双键,进一步脱氢交联后结焦成炭,起到阻隔作用。RGO具有催化成炭和物理阻隔作用,可以降低热释放速率,减少质量损失和延缓RPUF基体分解,复合材料热稳定性得到提高。
本发明在玻璃微珠表面包覆一层纳米TiO2薄膜,可以使其同时具备良好的隔热性能和高的近红外反射率,集阻隔隔热和反射隔热功能于一体。同时纳米TiO2薄膜外通过MDI修饰,将-NCO接枝到TiO2薄膜表面,当将其加入到发泡料中时,改性后的空心玻璃微珠能够参与到发泡反应中,与聚氨酯基体进行良好复合形成稳定的化学键,从而改善了复合材料的泡孔结构和物理性能。
本发明利用浸渍烧结的方法制备空心陶瓷纤维,继承了天然木棉纤维的中空管状结构,呈现中空微管状结构,拥有较高孔隙率,将其作为SO2凝胶的增强纤维,能够提高气凝胶纤维毡的隔热性能。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是本发明实施例3及对比例1~3中制备的单体电芯间的高效隔热阻燃材料缓冲层热重分析TG曲线。
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。
本发明公开了一种单体电芯间的高效隔热阻燃材料,包括芯层,所述芯层包是由二氧化硅气凝胶和空心陶瓷纤维复合的隔热纤维毡,所述芯层两侧包覆缓冲层,所述缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性的发泡聚氨酯,所述改性石墨烯为石墨烯经氧化还原后负载纳米氧化锌得到,所述改性空心玻璃微珠为玻璃微珠表面包覆纳米二氧化钛薄膜后接枝二苯基甲烷二异氰酸酯得到;
缓冲层包括以下重量份原料:聚醚多元醇4110 80~120份、石油醚3~5份、丙三醇1~3份、二月桂酸二丁基锡0.01~0.2份、二甲基环己胺0.1~0.5份、二苯基甲烷二异氰酸酯100~110份、改性石墨烯5~10份、改性空心玻璃微珠10~15分、聚磷酸铵1~3份、季戊四醇0.5~1.5份。
下面将结合实施例和对比例,对本发明单体电芯间的高效隔热阻燃材料进行清楚、完整地描述。
实施例1
一、原材料的制备和改性
1、空心陶瓷纤维的制备方法包括以下步骤:
将10.4g氯化铝及4.6g氯化镐溶解在120ml无水乙醇中,将3.5g木棉纤维浸入及氯化铝和氯化镐的混合溶液中,充分浸渍后取出挤干,并在80℃下干燥;再将干燥后的木棉纤维以3℃/min的升温速率加热到1000℃,保温2h,随炉冷却后即制得空心陶瓷纤维。
2、改性石墨烯的制备方法包括以下步骤:
A、先将1.2g石墨加入80ml浓H2SO4中并加热至85℃,使其与H2SO4发生反应,然后加入0.7gHNO3和5.8gKMnO4,进一步氧化石墨,形成氧化石墨烯,最后用水洗涤和离心分离,得到氧化石墨烯备用;
B、将1.5g氧化石墨烯加50ml入水中超声分散得到氧化石墨烯分散液,然后将30ml0.05~0.1mol/L的Zn(NO3)2溶液逐滴加入氧化石墨烯分散液中搅拌2h,最后用20%氨水调节pH值到10~11;
C、向混合液中加入0.5g NaBH4,密封后放入微波反应器内150℃反应10min,冷却过滤,用去离子水洗涤3~5次,80℃烘干得到改性石墨烯。
3、改性空心玻璃微珠的制备方法包括以下步骤:
S1、将10.3g空心玻璃微珠加入100ml 85℃饱和Ca(OH)2溶液中浸泡处理10h,然后用去离子水洗涤干燥,得到表面粗糙化的空心玻璃微珠,所选的空心玻璃微珠堆粒径为70~100μm,积密度为0.15~0.3g/cm3;
S2、将步骤S1处理后的空心玻璃微珠加入100ml 4wt%十二烷基苯磺酸钠水溶液中浸泡60min,烘干干燥得到表面活性剂处理的空心玻璃微珠;
S3、将步骤S2处理后的空心玻璃微珠加入80ml蒸馏水中搅拌均匀得到悬浊液,70℃下均匀滴加30ml 12wt%的Ti(SO4)2溶液,同时用20%氨水调节pH至恒定,反应结束后静置冷却抽滤,蒸馏水洗涤2~3次后烘干煅烧,得到纳米TiO2包覆的空心玻璃微珠;
S4、将步骤S3得到的纳米TiO2包覆的空心玻璃微珠粉末加入到100ml浓度为0.3mol/L的NaOH溶液中,75℃油浴锅中回流搅拌2h进行羟基化处理,然后减压抽滤同时用蒸馏水清洗玻璃微珠至其pH显中性,90℃真空干燥10h;
S5、将羟基化处理后的纳米TiO2包覆的空心玻璃微珠加入30%乙醇溶液中,然后向溶液中加入1.1g硅烷偶联剂KH550,80℃油浴锅中回流搅拌3h,用无水乙醇溶液进行反复洗涤、减压抽滤,100℃真空干燥10h;
S6、将步骤S5处理后的纳米TiO2包覆的空心玻璃微珠加入120ml N,N-二甲基甲酰胺中,再加入的3.4g二苯基甲烷二异氰酸酯,80℃油浴锅中回流搅拌2h,最后用N,N-二甲基甲酰胺反复洗涤、减压抽滤,100℃真空干燥10h,得到所述改性空心玻璃微珠。
二、单体电芯间的高效隔热阻燃材料芯层的制备
所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水按摩尔比1:7:3加入容器中混合搅拌3min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入空心陶瓷纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化12h;
(4)将老化后的复合材料按体积比1:2置于正己烷中进行溶剂交换12h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡12h,进行凝胶的表面基团改性,混合液中三甲基氯硅烷和正己烷体积比为1:8;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后80℃干燥8h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备
缓冲层各原料配比为:聚醚多元醇4110 115份、石油醚5份、丙三醇3份、二月桂酸二丁基锡0.2份、二甲基环己胺0.5份、二苯基甲烷二异氰酸酯110份、改性石墨烯10份、改性空心玻璃微珠14份、聚磷酸铵3份、季戊四醇1.3份
其制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合10min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10s;最后,将均匀混合的原料倒入模具合膜后置于45℃的烘箱中发泡1h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
四、单体电芯间的高效隔热阻燃材料的制备
将制备缓冲层包覆在芯层表面,可以通过在缓冲层内部开设容纳槽,将芯层填充在容纳槽中,也可以通过压敏胶水将缓冲层粘接在芯层表面,得到所述单体电芯间的高效隔热阻燃材料。
实施例2
一、空心陶瓷纤维、改性石墨烯、改性空心玻璃微珠的制备方法同实施例1。
二、单体电芯间的高效隔热阻燃材料芯层的制备
所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水按摩尔比1:7:3加入容器中混合搅拌3~5min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1~2h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入空心陶瓷纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化12~24h;
(4)将老化后的复合材料按体积比1:3置于正己烷中进行溶剂交换12~24h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡12h,进行凝胶的表面基团改性,混合液中三甲基氯硅烷和正己烷体积比为1:8~10;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后120℃干燥6h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备
缓冲层各原料配比为:聚醚多元醇4110 80份、石油醚3份、丙三醇1份、二月桂酸二丁基锡0.03份、二甲基环己胺0.1份、二苯基甲烷二异氰酸酯102份、改性石墨烯5份、改性空心玻璃微珠10份、聚磷酸铵1份、季戊四醇0.5份
其制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合6min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌25s;最后,将均匀混合的原料倒入模具合膜后置于40℃的烘箱中发泡2h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
四、单体电芯间的高效隔热阻燃材料的制备
将制备缓冲层包覆在芯层表面,可以通过在缓冲层内部开设容纳槽,将芯层填充在容纳槽中,也可以通过压敏胶水将缓冲层粘接在芯层表面,得到所述单体电芯间的高效隔热阻燃材料。
实施例3
一、空心陶瓷纤维、改性石墨烯、改性空心玻璃微珠的制备方法同实施例1。
二、单体电芯间的高效隔热阻燃材料芯层的制备
所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水按摩尔比1:7:3加入容器中混合搅拌4min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1.5h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入空心陶瓷纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化18h;
(4)将老化后的复合材料按体积比1:4置于正己烷中进行溶剂交换18h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡18h,进行凝胶的表面基团改性,混合液中三甲基氯硅烷和正己烷体积比为1:9;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后100℃干燥7h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备
缓冲层各原料配比为:聚醚多元醇4110 100份、石油醚4份、丙三醇2份、二月桂酸二丁基锡0.1份、二甲基环己胺0.3份、二苯基甲烷二异氰酸酯105份、改性石墨烯8份、改性空心玻璃微珠12份、聚磷酸铵2份、季戊四醇1份;
其制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合8min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10s;最后,将均匀混合的原料倒入模具合膜后置于42℃的烘箱中发泡1.5h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
四、单体电芯间的高效隔热阻燃材料的制备
将制备缓冲层包覆在芯层表面,可以通过在缓冲层内部开设容纳槽,将芯层填充在容纳槽中,也可以通过压敏胶水将缓冲层粘接在芯层表面,得到所述单体电芯间的高效隔热阻燃材料。
对比例1
一、改性石墨烯、改性空心玻璃微珠的制备方法同实施例1。
二、单体电芯间的高效隔热阻燃材料芯层的制备
本对比例中芯层采用二氧化硅气凝胶和玻璃纤维复合,所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水按摩尔比1:7:3加入容器中混合搅拌4min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1.5h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入玻璃纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化18h;
(4)将老化后的复合材料按体积比1:2~4置于正己烷中进行溶剂交换18h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡18h,进行凝胶的表面基团改性,混合液中三甲基氯硅烷和正己烷体积比为1:9;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后100℃干燥7h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备同实施例3。
对比例2
一、空心陶瓷纤维、改性空心玻璃微珠的制备方法同实施例1。
二、单体电芯间的高效隔热阻燃材料芯层的制备同实施例3。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备
在本对比例中,缓冲层由实施例1中步骤A制备的氧化石墨烯与改性空心玻璃微珠复合改性发泡聚氨酯,缓冲层各原料配比为:聚醚多元醇4110100份、石油醚4份、丙三醇2份、二月桂酸二丁基锡0.1份、二甲基环己胺0.3份、二苯基甲烷二异氰酸酯105份、氧化石墨烯8份、改性空心玻璃微珠12份、聚磷酸铵2份、季戊四醇1份;
其制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、氧化石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合8min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10s;最后,将均匀混合的原料倒入模具合膜后置于42℃的烘箱中发泡1.5h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
四、单体电芯间的高效隔热阻燃材料的制备
将制备缓冲层包覆在芯层表面,可以通过在缓冲层内部开设容纳槽,将芯层填充在容纳槽中,也可以通过压敏胶水将缓冲层粘接在芯层表面,得到所述单体电芯间的高效隔热阻燃材料。
对比例3
一、空心陶瓷纤维、改性空心玻璃微珠的制备方法同实施例1。
二、单体电芯间的高效隔热阻燃材料芯层的制备同实施例3。
三、单体电芯间的高效隔热阻燃材料缓冲层的制备
在本对比例中,缓冲层由改性石墨烯与未经过改性的空心玻璃微珠复合改性发泡聚氨酯,缓冲层各原料配比为:聚醚多元醇4110 100份、石油醚4份、丙三醇2份、二月桂酸二丁基锡0.1份、二甲基环己胺0.3份、二苯基甲烷二异氰酸酯105份、改性石墨烯8份、空心玻璃微珠12份、聚磷酸铵2份、季戊四醇1份;
其制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合8min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10s;最后,将均匀混合的原料倒入模具合膜后置于42℃的烘箱中发泡1.5h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
四、单体电芯间的高效隔热阻燃材料的制备
将制备缓冲层包覆在芯层表面,可以通过在缓冲层内部开设容纳槽,将芯层填充在容纳槽中,也可以通过压敏胶水将缓冲层粘接在芯层表面,得到所述单体电芯间的高效隔热阻燃材料。
性能检测
1、分别对实施例1~3以及对比例1~2制备的单体电芯间的高效隔热阻燃材料芯层、缓冲层通过导热系数测试仪测试常温下材料的导热系数,得到数据如下表1所示。
表1芯层、缓冲层常温下导热系数测试结果
由表1可以看出,本发明芯层的气凝胶纤维毡的常温导热系数在0.015~0.019W·m-1·K-1之间,本发明缓冲层的改性聚氨酯泡沫的常温导热系数在0.019~0.025之间,均具有超高的隔热性能。其中对比例1中芯层材料的增强纤维由空心陶瓷纤维替换为玻璃纤维,制得的芯层导热系数略微上升,达到0.024W·m-1·K-1,说明本发明空心陶瓷纤维拥有较高孔隙率,将其作为SO2凝胶的增强纤维,能够提高气凝胶纤维毡的隔热性能。对比例2和对比例3中分别采用了未改性氧化石墨烯和未改性的空心玻璃微珠,制得的缓冲层导热系数大幅上升,也直接证明改性石墨烯和改性空心玻璃微珠的加入,提高了聚氨酯泡沫的隔热性能。
2、将实施例3和对比例1~3制备的单体电芯间的高效隔热阻燃材料缓冲层进行热重分析,得到TG曲线如图1所示。
由图1可以看出,实施例3和对比例1中缓冲层的最大质量损失率温度相当,初始分解温度在350℃左右,对比例2和对比例3中的最大质量损失率温度低于实施例3,初始分解温度分别在280℃和300℃左右,说明本发明缓冲层中加入改性石墨烯、改性空心玻璃微珠提高了复合材料的热稳定性能。
3、将实施例1~3和对比例1~3制备的单体电芯间的高效隔热阻燃材料缓冲层进行垂直燃烧(UL94)测试,得到结果如表2所示。
表2缓冲层阻燃性能测试结果
由表2可以看出,本发明缓冲层的发泡聚氨酯的防火等级达V-0级,满足单体电芯间隔热阻燃材料的需求,其中对比例2中由于将改性石墨烯替换成了氧化石墨烯,缺少了ZnO与APP的协效阻燃,因此制备的缓冲层防火等级略低。
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。
Claims (10)
1.一种单体电芯间的高效隔热阻燃材料,其特征在于,包括芯层,所述芯层是由二氧化硅气凝胶和空心陶瓷纤维复合的隔热纤维毡,所述芯层两侧包覆缓冲层,所述缓冲层是由改性石墨烯、改性空心玻璃微珠复合改性的发泡聚氨酯,所述改性石墨烯为石墨烯经氧化还原后负载纳米氧化锌得到,所述改性空心玻璃微珠为玻璃微珠表面包覆纳米二氧化钛薄膜后接枝二苯基甲烷二异氰酸酯得到;
所述缓冲层包括以下重量份原料:聚醚多元醇411080~120份、石油醚3~5份、丙三醇1~3份、二月桂酸二丁基锡0.01~0.2份、二甲基环己胺0.1~0.5份、二苯基甲烷二异氰酸酯100~110份、改性石墨烯5~10份、改性空心玻璃微珠10~15分、聚磷酸铵1~3份、季戊四醇0.5~1.5份。
2.根据权利要求1所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述芯层的制备方法包括以下步骤:
(1)将正硅酸乙酯、无水乙醇和去离子水加入容器中混合搅拌3~5min,然后加入1.0mol/L盐酸调节pH为2~3,搅拌水解1~2h,得到硅溶胶;
(2)将0.5mol/L氨水慢速加入到硅溶胶中,边滴加边搅拌至pH为7~8,然后将硅溶胶迅速倒入空心陶瓷纤维毡预制件中直至刚好淹没纤维毡为止,静置凝胶;
(3)将凝胶后的复合材料置于容器中,加入无水乙醇,室温下老化12~24h;
(4)将老化后的复合材料按体积比1:2~4置于正己烷中进行溶剂交换12~24h,置换出凝胶骨架中残留的去离子水;
(5)将溶剂交换完毕的湿复合材料于三甲基氯硅烷和正己烷的混合液中浸泡12~24h,进行凝胶的表面基团改性;
(6)最后,将步骤(5)制得的复合材料进行正己烷清洗表面,然后80~120℃干燥6~8h,得到疏水型二氧化硅气凝胶复合纤维毡芯层。
3.根据权利要求2所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述步骤(1)中正硅酸乙酯、无水乙醇和去离子水按摩尔比为1:7:3。
4.根据权利要求2所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述步骤(5)中三甲基氯硅烷和正己烷的体积比为1:8~10。
5.根据权利要求2所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述空心陶瓷纤维的制备方法包括以下步骤:
先将木棉纤维浸入氯化铝及氯化镐的乙醇溶液中,充分浸渍后取出挤干,并在60~80℃下干燥;再将干燥后的木棉纤维以2~4℃/min的升温速率加热到800~1200℃,保温1~3h,随炉冷却后即制得空心陶瓷纤维。
6.根据权利要求5所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述氯化铝及氯化镐的乙醇溶液中氯化铝及氯化镐的摩尔比为3~5:1。
7.根据权利要求1所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述缓冲层的制备方法包括以下步骤:
将聚醚多元醇4110、石油醚、丙三醇、二月桂酸二丁基锡、二甲基环己胺、改性石墨烯、改性空心玻璃微珠、聚磷酸铵、季戊四醇按比例搅拌混合5~10min,使各原料混合均匀;然后迅速加入二苯基甲烷二异氰酸酯,快速搅拌10~30s;最后,将均匀混合的原料倒入模具合膜后置于40~45℃的烘箱中发泡1~2h,发泡完成后模具随炉冷却至室温脱模,得到发泡聚氨酯缓冲层。
8.根据权利要求6所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述改性石墨烯的制备方法包括以下步骤:
A、先将石墨加入浓H2SO4中并加热至80~90℃,使其与H2SO4发生反应,然后加入HNO3和KMnO4,进一步氧化石墨,形成氧化石墨烯,最后用水洗涤和离心分离,得到氧化石墨烯备用;
B、将氧化石墨烯加入水中超声分散得到氧化石墨烯分散液,然后将0.05~0.1mol/L的Zn(NO3)2溶液逐滴加入氧化石墨烯分散液中搅拌1~3h,最后用20%氨水调节pH值到10~11;
C、向混合液中加入NaBH4,密封后放入微波反应器内140~160℃反应8~10min,冷却过滤,用去离子水洗涤3~5次,70~80℃烘干得到改性石墨烯。
9.根据权利要求6所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述改性空心玻璃微珠的制备方法包括以下步骤:
S1、将空心玻璃微珠加入80~90℃饱和Ca(OH)2溶液中浸泡处理8~10h,然后用去离子水洗涤干燥,得到表面粗糙化的空心玻璃微珠;
S2、将步骤S1处理后的空心玻璃微珠加入3~5wt%十二烷基苯磺酸钠水溶液中浸泡30~90min,烘干干燥得到表面活性剂处理的空心玻璃微珠;
S3、将步骤S2处理后的空心玻璃微珠加入蒸馏水中搅拌均匀得到悬浊液,60~80℃下均匀滴加10~15wt%的Ti(SO4)2溶液,同时用20%氨水调节pH至恒定,反应结束后静置冷却抽滤,蒸馏水洗涤2~3次后烘干煅烧,得到纳米TiO2包覆的空心玻璃微珠;
S4、将步骤S3得到的纳米TiO2包覆的空心玻璃微珠粉末加入到浓度为0.3mol/L的NaOH溶液中,70~80℃油浴锅中回流搅拌1~3h进行羟基化处理,然后减压抽滤同时用蒸馏水清洗玻璃微珠至其pH显中性,80~100℃真空干燥8~12h;
S5、将羟基化处理后的纳米TiO2包覆的空心玻璃微珠加入30%乙醇溶液中,然后向溶液中加入硅烷偶联剂KH550,70~80℃油浴锅中回流搅拌2~4h,用无水乙醇溶液进行反复洗涤、减压抽滤,80~100℃真空干燥8~12h;
S6、将步骤S5处理后的纳米TiO2包覆的空心玻璃微珠加入N,N-二甲基甲酰胺中,再加入的二苯基甲烷二异氰酸酯,70~80℃油浴锅中回流搅拌1~3h,最后用N,N-二甲基甲酰胺反复洗涤、减压抽滤,80~100℃真空干燥8~12h,得到所述改性空心玻璃微珠。
10.根据权利要求9所述的单体电芯间的高效隔热阻燃材料,其特征在于,所述空心玻璃微珠堆粒径为70~100μm,积密度为0.15~0.3g/cm3。
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