CN117429133B - 一种耐高低温的弹性隔热板及其制备工艺 - Google Patents

一种耐高低温的弹性隔热板及其制备工艺 Download PDF

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CN117429133B
CN117429133B CN202311375956.5A CN202311375956A CN117429133B CN 117429133 B CN117429133 B CN 117429133B CN 202311375956 A CN202311375956 A CN 202311375956A CN 117429133 B CN117429133 B CN 117429133B
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heat insulation
film
minutes
calcium silicate
container
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CN117429133A (zh
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梁玲玲
周伯韬
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Utson New Material Group Co ltd
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Utson New Material Group Co ltd
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Abstract

本发明涉及建筑材料技术领域,具体地说是一种耐高低温的弹性隔热板及其制备工艺。一种耐高低温的弹性隔热板及其制备工艺,包括以下步骤:隔热基板的制作;PDMS预混粘结剂和溶剂型丙烯酸酯的制备;间隔板的制备;制备反射复合膜;隔热基板的覆膜与粘合。本发明先通过对硅酸钙进行发泡处理,使硅酸钙能够获得高强度的压缩、弯曲能力,吸收更多的能量,具备良好的弹性,然后再通过将发泡硅酸钙制成球形,与PDMS预混粘结剂混合,球与球之间能实现较大转动,进一步增加材料的弹性,综上所述,间隔板与同样具有良好的弹性的隔热基板粘合在一起,制得的隔热板具有更大的弹性,并且在获得更好的隔热能力的同时又不缺失强度。

Description

一种耐高低温的弹性隔热板及其制备工艺
技术领域
本发明涉及建筑材料技术领域,具体地说是一种耐高低温的弹性隔热板及其制备工艺。
背景技术
隔热板是一种用于隔离热量传递和提供隔热保护的材料,它们通常由具有优异绝热性能的材料制成,广泛用于建筑、工业和航空航天等领域。
在建筑的墙体、屋顶和地板等部位安装隔热板可以有效减少能量损失和热巧效应,提高建筑保温性能;在锅炉、管道、储罐、炉窖等工业设备上,也经常需要安装隔热板进行保温处理,提高设备的工作效率和节能效果;在冷库和制冷设备中,隔热板又能隔离内外温度,确保冷冻和冷藏物品的稳定温度。
隔热板在许多领域都发挥着重要作用,但在这些领域中的隔热板往往只拥有耐热或者耐寒的特性,导致在不同环境下需要更换不同类型的隔热板,且部分隔热板的弹性不好,例如聚氨酯泡沫板,容易在使用过程中发生断裂。
为解决上述工艺难点,本发明提供了一种耐高低温的弹性隔热板及其制备工艺。
发明内容
为了解决上述技术缺陷,本发明提供了一种耐高低温的弹性隔热板及其制备工艺。
一种耐高低温的弹性隔热板的制备工艺,具体包括以下步骤:
S1:隔热基板的制作
将硅酸铝纤维进行超声分散之后与聚丙烯酰胺、去离子水、铝溶胶、硅酸钙混合搅拌,再对混合液进行超声分散,然后投入循环水真空泵中真空抽滤,得到硅酸钙/硅酸铝纤维复合材料,备用;
S2:PDMS预混粘结剂和溶剂型丙烯酸酯的制备
将聚二甲基硅氧烷与固化剂混合、干燥固化、均匀分散制得PDMS预混粘结剂,将丙烯酸丁酯、水溶性聚乙烯醇和丁烯二酸混合,得到混合液,将蒸馏水和十二烷基苯磺酸钙盐加入烧瓶加热,再加入混合液、过硫酸铵和非离子表面活性剂,持续加热反应,冷却后与松香皂混合得到溶剂型丙烯酸酯;
进一步地,步骤S2中的松香皂由松香、烧碱和水混合加热之后冷却制得;
S3:间隔板的制备
将固态硅酸钙熔融,加入增粘剂搅拌,再加入发泡剂TiH2搅拌,将发泡的熔体加入熔融造粒机中造粒,得到球形孔发泡硅酸钙球粒,将球形孔发泡硅酸钙球粒与PDMS预混粘结剂混合、均匀分散、压缩,制得间隔板,备用;
S4:制备反射复合膜
将铝丝通过真空蒸镀机蒸镀在BOPP塑料薄膜上,得到镀铝膜成品,将溶剂型粘合剂丙烯酸酯涂在镀铝膜成品表面,在覆膜机中通过热合法使PET膜粘结在镀铝膜成品表面,得到反射复合膜,备用;
S5:隔热基板的覆膜与粘合
将隔热基板一面涂上溶剂型丙烯酸酯,在覆膜机中通过热合法使反射复合膜粘结在隔热基板涂有溶剂型丙烯酸酯的一面上,得到覆膜隔热基板,取两块覆膜隔热基板在未覆膜一面涂上PDMS预混粘结剂,将间隔板置于两块覆膜隔热基板之间,加热压缩,制得一种耐高低温的弹性隔热板。
进一步地,步骤S1隔热基板的制作,具体包括以下步骤:
S1.1:将3-4份硅酸铝纤维置于4-5份去离子水中,然后过60-80目筛制得硅酸铝纤维浆,将浓度为0.4-0.6%的硅酸铝纤维浆和浓度为0.6-0.8%的聚丙烯酰胺分散剂按3:(2-2.5)的比例混合,然后置于超声波乳化分散机进行超声分散6-8分钟,得到改性硅酸铝纤维,备用;
S1.2:将浓度为0.6-0.8%的聚丙烯酰胺、去离子水、铝溶胶、硅酸钙和改性硅酸铝纤维以1:(2.5-3):(0.1-0.2):(0.5-1):(3-4)的质量比混合,投入叶片式搅拌机中搅拌5-6分钟,再将所得混合液投入超声波乳化分散机,进行超声分散6-8分钟,再投入循环水真空泵中真空抽滤10-12分钟,得到硅酸钙/硅酸铝纤维复合材料,备用;
S1.3:将1-1.5cm的垫片置于模压机底部,随后将硅酸钙/硅酸铝纤维复合材料投入模压机中以100-110℃压印10-15分钟,制得隔热基板,备用。
进一步地,步骤S2PDMS预混粘结剂和溶剂型丙烯酸酯的制备,具体包括以下步骤:
S2.1:将聚二甲基硅氧烷与固化剂按照(10-15):1的质量比混合,随后置于烘干箱中以75-80℃的温度固化3-5分钟,然后将固化后的聚二甲基硅氧烷基体与硅酸钙颗粒和硅酸纤维以1:(3-3.5):(1.5-2)的质量比进行混合,再将所得混合物投入非介入式材料均质机中,调节转速为2000-2100rpm,均匀分散2-3分钟,制成PDMS预混粘结剂,备用;
S2.2:将2-3份丙烯酸丁酯、2-3份水溶性聚乙烯醇和0.25-0.3份丁烯二酸混合均匀,得到混合液,随后将3-5份蒸馏水和0.04-0.05份十二烷基苯磺酸钙盐加入容器中,容器加热至75-80℃,然后加入0.3-0.35份过硫酸铵、0.1-0.2份聚氧乙烯型非离子表面活性剂和0.2-0.3份混合液,静置10-15分钟后,向容器内缓慢滴加1.8-2.7份混合液,然后再加入0.2-0.3份过硫酸铵,容器持续加热使温度保持在75-80℃,静置25-30分钟,随后自然降温10-15分钟,使温度降至40-50℃,得到混合乳液,备用;
S2.3:将0.5-1份松香、0.05-0.1份烧碱和5-6份水装入三口烧瓶中,加热至80-120℃反应2-3小时,然后自然降温25-30分钟,使温度降至50-60℃,得到松香皂,将所得的1-2份松香皂加入4-5份乳液中混合搅拌15-20分钟,得到溶剂型丙烯酸酯,备用。
进一步地,步骤S3间隔板的制备,具体包括以下步骤:
S3.1:将4-5份固态硅酸钙置于容器中,再将坩埚置于高温电炉中,调节温度为1600-1800℃熔融25-30分钟,随后加入粒径为2-3mm的增粘剂0.2-0.3份搅拌15-20分钟,然后加入0.01-0.04份发泡剂TiH2搅拌2-3分钟,在1600-1800℃温度下静置1-2分钟后将坩埚取出,将坩埚内的硅酸钙熔体倒入熔融造粒机中,调节制造粒径为1-1.5cm,直到硅酸钙熔体全部造粒完成,得到球形孔发泡硅酸钙球粒,备用;
S3.2:将步骤S2.1中制得的PDMS预混粘结剂与发泡硅酸钙球粒以1:(2-2.5)的质量比混合,将所得混合物投入非介入式材料均质机,调节转速为1900-2000rpm,均匀分散1-2分钟,再将均匀分散的混合物置入模压机中,调节温度为100-105℃,压缩10-15分钟,制得间隔板;
S3.3:将0.5-0.7份PDMS预混粘结剂均匀涂于隔热层的上下两面,随后置于模压机中,调节温度为100-110℃,压力为15-20Mpa,压缩10-15分钟,得到间隔板。
进一步地,步骤S4制备反射复合膜,具体包括以下步骤:
S4.1:将BOPP塑料薄膜装于真空蒸镀机中,再将纯度为99.9%以上的铝丝1-1.5份置于蒸镀机的坩埚中,启动真空泵使蒸镀机中的真空度达到1.3×10-3~1.3×10-2Pa,并启动加热器,使坩埚温度为1200-1400℃,控制BOPP塑料薄膜的移动速度为170-180m/分钟,并将铝丝镀在BOPP塑料薄膜表面,得到厚度为60-70nm的镀铝膜,随后打开冷却装置将镀铝膜冷却至55-60℃,然后取出自然冷却,得到镀铝膜成品;
S4.2:将1-2份溶剂型粘合剂丙烯酸酯均匀地涂在镀铝膜成品表面,使镀铝膜成品表面的上浆量为9-12g/m2,随后将其与两张6-8mm的PET膜置于覆膜机中,调节覆膜机烘道温度为55-60℃,加热辊的温度为110-120℃,加热辊卷绕线速度为6-8m/分钟,上卷张力为29.4-31.6N,经过1-2分钟,使镀铝膜成品两面均粘结上PET膜,得到反射复合膜,备用。
进一步地,步骤S5隔热基板的覆膜与粘合,具体包括以下步骤:
S5.1:将隔热基板一面均匀地涂上0.5-1份步骤S2.3制备的溶剂型丙烯酸酯,使隔热基板一面的上浆量为9-12g/m2,将其与反射复合膜置入覆膜机中,调节覆膜机烘道温度为55-60℃,加热辊的温度为110-120℃,加热辊卷绕线速度为3-5m/分钟,上卷张力为32.5-33.7N,经过2-3分钟,得到覆膜隔热基板,备用;
S5.2:取两块覆膜隔热基板,均在未覆膜的一面均匀涂上0.5-0.7份步骤S2.1制备的PDMS预混粘结剂,将间隔板至于两块隔热基板之间,间隔板上下两面分别与覆膜隔热基板涂有PDMS预混粘结剂的一面接触,随后置于模压机中并启动模压机,调节模压机温度为100-110℃,压力为10-15Mpa,压缩10-15分钟,得到一种耐高低温的弹性隔热板。
进一步地,步骤S3.1中的增粘剂为硅胶增粘剂。
进一步地,步骤S2.2的容器底部设有重力传感器,重力传感器可以控制容器底部的加热装置启动与关闭,当向容器中加入蒸馏水和十二烷基苯磺酸钙盐时,重力传感器感应到容器内重量增加发出信号,信号被加热装置上的控制器就接收从而启动加热装置,使容器温度达到75-80℃,再加入过硫酸铵、聚氧乙烯型非离子表面活性剂和混合液,重力传感器再次感应到容器内质量增加,使加热装置继续加热,容器温度达到75-80℃没有物质通过时,控制器控制加热装置停止加热,静置10-15分钟后,向容器内缓慢滴加混合液,重力传感器感应到重量持续增加并发出信号,信号被控制器接收启动加热装置,使温度一直维持在75-80℃,当滴加完混合液后,信号消失,控制器控制加热装置关闭。
一种耐高低温的弹性隔热板,其由一种耐高低温的弹性隔热板的制备工艺制备得到。
有益效果是:1、本发明先通过对硅酸钙进行发泡处理,使硅酸钙能够获得高强度的压缩、弯曲能力,吸收更多的能量,具备良好的弹性,然后再通过将发泡硅酸钙制成球形,与PDMS预混粘结剂混合,球与球之间能实现较大转动,进一步增加材料的弹性,综上所述,间隔板与同样具有良好的弹性的隔热基板粘合在一起,制得的隔热板具有更大的弹性,并且在获得更好的隔热能力的同时又不缺失强度。
2、本发明通过将丙烯酸丁酯、水溶性聚乙烯醇和丁烯二酸为主要成分制作一种溶剂型丙烯酸酯粘结剂,其中丙烯酸丁酯能够使粘结剂热合之后形成的膜具备优良的粘性,水溶性聚乙烯醇可以使粘结剂在热合时更好的形成薄膜,还能进一步增加膜的粘结能力并使成形的膜具有较低的热导率,丁烯二酸具有高透明度、耐热性和高稳定性等特点,在粘合剂中作为功能单体,可提高乳液的耐热性和稳定性,使用这种溶剂型丙烯酸酯粘结剂能够使隔热板各部分紧密结合,防止材料在发生形变时发生相对移动,使隔热板保持良好的弹性,同时还能够增强隔热板的隔热能力。
3、本发明先将硅酸钙和硅酸铝纤维混合后进行超声分散,制得具备良好的柔性的硅酸钙/硅酸铝纤维复合材料,再通过压缩将硅酸钙/硅酸铝纤维复合材料制成隔热基板,使隔热基板具备良好的弹性,又由于硅酸钙、硅酸铝纤维均具备优秀的耐高低温性能,隔热基板在隔热板最外层时,使隔热板获得优秀的耐高低温性。
4、本发明通过在容器口安装重力传感器,当有物质加入容器内时,加热装置自动启动,使容器内的反应能够进行,当持续向容器内滴加混合液时,容器能保持反应需要的温度,使反应精准,顺利地进行,对人们来说省时省力。
附图说明
图1为本发明的实施例所采用的一种耐高低温的弹性隔热板的制备工艺流程图。
图2为本发明的对比例1中耐高低温的弹性隔热板与硅酸钙板在不同温度下导热系数的对比表格图。
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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种耐高低温的弹性隔热板及其制备工艺,如图1所示,具体包括以下步骤:
S1:隔热基板的制作
S1.1:将3份硅酸铝纤维置于4份去离子水中,然后过60目筛制,使硅酸铝纤维中的渣球含量大幅降低,得硅酸铝纤维浆,将浓度为0.4%的硅酸铝纤维浆和浓度为0.6%的聚丙烯酰胺分散剂按3:2的比例混合,然后置于超声波乳化分散机进行超声分散6分钟,得到改性硅酸铝纤维,备用;
S1.2:将浓度为0.6%的聚丙烯酰胺、去离子水、铝溶胶、硅酸钙和改性硅酸铝纤维以1:2.5:0.2:1:4的质量比混合,硅酸钙、硅酸铝纤维均具备优秀的耐高低温性能,投入叶片式搅拌机中搅拌5分钟,再将所得混合液投入超声波乳化分散机,进行超声分散6分钟,使后续制备的硅酸钙/硅酸铝纤维复合材料获得更好的柔性,再投入循环水真空泵中真空抽滤10分钟,得到硅酸钙/硅酸铝纤维复合材料,备用;
S1.3:将1cm的垫片置于模压机底部,使压缩时隔热基板厚度控制在1cm,随后将硅酸钙/硅酸铝纤维复合材料投入模压机中以100℃压印10分钟,制得隔热基板,备用。
S2:PDMS预混粘结剂和溶剂型丙烯酸酯的制备
S2.1:将聚二甲基硅氧烷与固化剂按照10:1的质量比混合,随后置于烘干箱中以75℃的温度固化3分钟,然后将固化后的聚二甲基硅氧烷基体与硅酸钙颗粒和硅酸纤维以1:3:1.5的质量比进行混合,再将所得混合物投入非介入式材料均质机中,调节转速为2000rpm,均匀分散2分钟,制成PDMS预混粘结剂,备用;
S2.2:将2份丙烯酸丁酯、2份水溶性聚乙烯醇和0.25份丁烯二酸混合均匀,丙烯酸丁酯能够使粘结剂热合之后形成的膜具备优良的粘性,水溶性聚乙烯醇可以使粘结剂在热合时更好的形成薄膜,还能进一步增加膜的粘结能力并使成形的膜具有较低的热导率,丁烯二酸具有高透明度、耐热性和高稳定性等特点,在粘合剂中作为功能单体,可提高乳液的耐热性和稳定性,得到混合液,随后将3份蒸馏水和0.04份十二烷基苯磺酸钙盐加入容器中,容器加热至75℃,然后加入0.3份过硫酸铵、0.1份聚氧乙烯型非离子表面活性剂和0.2份混合液,静置10分钟后,向容器内缓慢滴加1.8份混合液,然后再加入0.2份过硫酸铵,容器持续加热使温度保持在75℃,静置25分钟,随后自然降温10分钟,使温度降至40℃,得到混合乳液,备用;
S2.3:将0.5份松香、0.05份烧碱和5份水装入三口烧瓶中,加热至80℃反应2小时,然后自然降温25分钟,使温度降至50℃,得到松香皂,将所得的1份松香皂加入4份乳液中混合搅拌15分钟,得到溶剂型丙烯酸酯,备用。
S3:间隔板的制备
S3.1:将4份固态硅酸钙置于容器中,再将坩埚置于高温电炉中,调节温度为1600℃熔融25分钟,随后加入粒径为2mm的增粘剂0.2份搅拌15分钟,然后加入0.01份发泡剂TiH2搅拌2分钟,对硅酸钙进行发泡处理,使硅酸钙能够获得高强度的压缩、弯曲能力,吸收更多的能量,具备良好的弹性,在1600℃温度下静置1分钟后将坩埚取出,将坩埚内的硅酸钙熔体倒入熔融造粒机中,调节制造粒径为1cm,直到硅酸钙熔体全部造粒完成,得到球形孔发泡硅酸钙球粒,球与球之间能实现较大转动,备用;
S3.2:将步骤S2.1中制得的PDMS预混粘结剂与发泡硅酸钙球粒以1:2的质量比混合,进一步增加材料的弹性,将所得混合物投入非介入式材料均质机,调节转速为1900rpm,均匀分散1分钟,再将均匀分散的混合物置入模压机中,调节温度为100℃,压缩10分钟,制得间隔板;
S3.3:将0.5份PDMS预混粘结剂均匀涂于隔热层的上下两面,随后置于模压机中,调节温度为100℃,压力为15Mpa,压缩10分钟,使隔热层上下两面生成封装层,进一步使间隔板的柔性与隔热性能得到提升,得到间隔板。
S4:制备反射复合膜
S4.1:将BOPP塑料薄膜装于真空蒸镀机中,再将纯度为99.9%以上的铝丝1份置于蒸镀机的坩埚中,启动真空泵使蒸镀机中的真空度达到1.3×10-3Pa,并启动加热器,使坩埚温度为1200℃,使铝丝气态化,控制BOPP塑料薄膜的移动速度为170m/分钟,并将铝丝镀在BOPP塑料薄膜表面,得到厚度为60nm的镀铝膜,随后打开冷却装置将镀铝膜冷却至55℃,然后取出自然冷却,得到镀铝膜成品;
S4.2:将1份溶剂型粘合剂丙烯酸酯均匀地涂在镀铝膜成品表面,使镀铝膜成品表面的上浆量为9g/m2,随后将其与两张6mm的PET膜置于覆膜机中,调节覆膜机烘道温度为55℃,加热辊的温度为110℃,加热辊卷绕线速度为8m/分钟,上卷张力为29.4N,经过1分钟,使镀铝膜成品两面均粘结上PET膜,覆膜机烘道首先对溶剂型粘合剂丙烯酸酯干燥除去溶剂,覆膜机再将表面干燥的镀铝膜成品送入加热辊,与PET膜相遇,镀铝膜与PET膜在热压状态下被粘合,得到反射复合膜,备用。
S5:隔热基板的覆膜与粘合
S5.1:将隔热基板一面均匀地涂上0.5份步骤S2.3制备的溶剂型丙烯酸酯,使用这种溶剂型丙烯酸酯粘结剂能够使隔热板各部分紧密结合,防止材料在发生形变时发生相对移动,使隔热板保持良好的弹性,同时还能够增强隔热板的隔热能力,使隔热基板一面的上浆量为9g/m2,将其与反射复合膜置入覆膜机中,调节覆膜机烘道温度为55℃,加热辊的温度为110℃,加热辊卷绕线速度为5m/分钟,上卷张力为32.5N,经过2分钟,得到覆膜隔热基板,备用;
S5.2:取两块覆膜隔热基板,均在未覆膜的一面均匀涂上0.5份步骤S2.1制备的PDMS预混粘结剂,将间隔板至于两块隔热基板之间,间隔板上下两面分别与覆膜隔热基板涂有PDMS预混粘结剂的一面接触,随后置于模压机中并启动模压机,调节模压机温度为100℃,压力为10Mpa,压缩10分钟,得到一种耐高低温的弹性隔热板,间隔板与同样具有良好的弹性的隔热基板粘合在一起,制得的隔热板具有更大的弹性,并且在获得更好的隔热能力的同时又不缺失强度。
S2.2的容器底部设有重力传感器,重力传感器可以控制容器底部的加热装置启动与关闭,当向容器中加入蒸馏水和十二烷基苯磺酸钙盐时,重力传感器感应到容器内重量增加发出信号,信号被加热装置上的控制器就接收从而启动加热装置,使容器温度达到75℃,再加入过硫酸铵、聚氧乙烯型非离子表面活性剂和混合液,重力传感器再次感应到容器内质量增加,使加热装置继续加热,容器温度达到75℃没有物质通过时,控制器控制加热装置停止加热,静置10分钟后,向容器内缓慢滴加混合液,重力传感器感应到重量持续增加并发出信号,信号被控制器接收启动加热装置,使温度一直维持在75℃,当滴加完混合液后,信号消失,控制器控制加热装置关闭。
实施例2
一种耐高低温的弹性隔热板及其制备工艺,如图1所示,具体包括以下步骤:
S1:隔热基板的制作
S1.1:将4份硅酸铝纤维置于5份去离子水中,然后过60目筛制,使硅酸铝纤维中的渣球含量大幅降低,得硅酸铝纤维浆,将浓度为0.6%的硅酸铝纤维浆和浓度为0.8%的聚丙烯酰胺分散剂按3:2.5的比例混合,然后置于超声波乳化分散机进行超声分散6分钟,得到改性硅酸铝纤维,备用;
S1.2:将浓度为0.8%的聚丙烯酰胺、去离子水、铝溶胶、硅酸钙和改性硅酸铝纤维以1:3:0.1:0.5:3的质量比混合,硅酸钙、硅酸铝纤维均具备优秀的耐高低温性能,投入叶片式搅拌机中搅拌5分钟,再将所得混合液投入超声波乳化分散机,进行超声分散6分钟,使后续制备的硅酸钙/硅酸铝纤维复合材料获得更好的柔性,再投入循环水真空泵中真空抽滤10分钟,得到硅酸钙/硅酸铝纤维复合材料,备用;
S1.3:将1cm的垫片置于模压机底部,使压缩时隔热基板厚度控制在1cm,随后将硅酸钙/硅酸铝纤维复合材料投入模压机中以100℃压印10分钟,制得隔热基板,备用。
S2:PDMS预混粘结剂和溶剂型丙烯酸酯的制备
S2.1:将聚二甲基硅氧烷与固化剂按照15:1的质量比混合,随后置于烘干箱中以75℃的温度固化3分钟,然后将固化后的聚二甲基硅氧烷基体与硅酸钙颗粒和硅酸纤维以1:3.5:2的质量比进行混合,再将所得混合物投入非介入式材料均质机中,调节转速为2000rpm,均匀分散2分钟,制成PDMS预混粘结剂,备用;
S2.2:将3份丙烯酸丁酯、3份水溶性聚乙烯醇和0.3份丁烯二酸混合均匀,丙烯酸丁酯能够使粘结剂热合之后形成的膜具备优良的粘性,水溶性聚乙烯醇可以使粘结剂在热合时更好的形成薄膜,还能进一步增加膜的粘结能力并使成形的膜具有较低的热导率,丁烯二酸具有高透明度、耐热性和高稳定性等特点,在粘合剂中作为功能单体,可提高乳液的耐热性和稳定性,得到混合液,随后将5份蒸馏水和0.05份十二烷基苯磺酸钙盐加入容器中,容器加热至75℃,然后加入0.35份过硫酸铵、0.2份聚氧乙烯型非离子表面活性剂和0.3份混合液,静置10分钟后,向容器内缓慢滴加2.7份混合液,然后再加入0.3份过硫酸铵,容器持续加热使温度保持在75℃,静置25分钟,随后自然降温10分钟,使温度降至40℃,得到混合乳液,备用;
S2.3:将1份松香、0.1份烧碱和6份水装入三口烧瓶中,加热至80℃反应2小时,然后自然降温25分钟,使温度降至50℃,得到松香皂,将所得的2份松香皂加入5份乳液中混合搅拌15分钟,得到溶剂型丙烯酸酯,备用。
S3:间隔板的制备
S3.1:将4份固态硅酸钙置于容器中,再将坩埚置于高温电炉中,调节温度为1600℃熔融25分钟,随后加入粒径为3mm的增粘剂0.3份搅拌15分钟,然后加入0.03份发泡剂TiH2搅拌2分钟,对硅酸钙进行发泡处理,使硅酸钙能够获得高强度的压缩、弯曲能力,吸收更多的能量,具备良好的弹性,在1600℃温度下静置1分钟后将坩埚取出,将坩埚内的硅酸钙熔体倒入熔融造粒机中,调节制造粒径为1.5cm,直到硅酸钙熔体全部造粒完成,得到球形孔发泡硅酸钙球粒,球与球之间能实现较大转动,备用;
S3.2:将步骤S2.1中制得的PDMS预混粘结剂与发泡硅酸钙球粒以1:2.5的质量比混合,进一步增加材料的弹性,将所得混合物投入非介入式材料均质机,调节转速为1900rpm,均匀分散1分钟,再将均匀分散的混合物置入模压机中,调节温度为100℃,压缩10分钟,制得间隔板;
S3.3:将0.7份PDMS预混粘结剂均匀涂于隔热层的上下两面,随后置于模压机中,调节温度为100℃,压力为15Mpa,压缩10分钟,使隔热层上下两面生成封装层,进一步使间隔板的柔性与隔热性能得到提升,得到间隔板。
S4:制备反射复合膜
S4.1:将BOPP塑料薄膜装于真空蒸镀机中,再将纯度为99.9%以上的铝丝1.5份置于蒸镀机的坩埚中,启动真空泵使蒸镀机中的真空度达到1.3×10-3Pa,并启动加热器,使坩埚温度为1200℃,使铝丝气态化,控制BOPP塑料薄膜的移动速度为170m/分钟,并将铝丝镀在BOPP塑料薄膜表面,得到厚度为60nm的镀铝膜,随后打开冷却装置将镀铝膜冷却至55℃,然后取出自然冷却,得到镀铝膜成品;
S4.2:将2份溶剂型粘合剂丙烯酸酯均匀地涂在镀铝膜成品表面,使镀铝膜成品表面的上浆量为10g/m2,随后将其与两张8mm的PET膜置于覆膜机中,调节覆膜机烘道温度为55℃,加热辊的温度为110℃,加热辊卷绕线速度为8m/分钟,上卷张力为29.4N,经过1分钟,使镀铝膜成品两面均粘结上PET膜,覆膜机烘道首先对溶剂型粘合剂丙烯酸酯干燥除去溶剂,覆膜机再将表面干燥的镀铝膜成品送入加热辊,与PET膜相遇,镀铝膜与PET膜在热压状态下被粘合,得到反射复合膜,备用。
S5:隔热基板的覆膜与粘合
S5.1:将隔热基板一面均匀地涂上1份步骤S2.3制备的溶剂型丙烯酸酯,使用这种溶剂型丙烯酸酯粘结剂能够使隔热板各部分紧密结合,防止材料在发生形变时发生相对移动,使隔热板保持良好的弹性,同时还能够增强隔热板的隔热能力,使隔热基板一面的上浆量为12g/m2,将其与反射复合膜置入覆膜机中,调节覆膜机烘道温度为55℃,加热辊的温度为110℃,加热辊卷绕线速度为5m/分钟,上卷张力为32.5N,经过2分钟,得到覆膜隔热基板,备用;
S5.2:取两块覆膜隔热基板,均在未覆膜的一面均匀涂上0.7份步骤S2.1制备的PDMS预混粘结剂,将间隔板至于两块隔热基板之间,间隔板上下两面分别与覆膜隔热基板涂有PDMS预混粘结剂的一面接触,随后置于模压机中并启动模压机,调节模压机温度为100℃,压力为10Mpa,压缩10分钟,得到一种耐高低温的弹性隔热板,间隔板与同样具有良好的弹性的隔热基板粘合在一起,制得的隔热板具有更大的弹性,并且在获得更好的隔热能力的同时又不缺失强度。
S2.2的容器底部设有重力传感器,重力传感器可以控制容器底部的加热装置启动与关闭,当向容器中加入蒸馏水和十二烷基苯磺酸钙盐时,重力传感器感应到容器内重量增加发出信号,信号被加热装置上的控制器就接收从而启动加热装置,使容器温度达到75℃,再加入过硫酸铵、聚氧乙烯型非离子表面活性剂和混合液,重力传感器再次感应到容器内质量增加,使加热装置继续加热,容器温度达到75℃没有物质通过时,控制器控制加热装置停止加热,静置10分钟后,向容器内缓慢滴加混合液,重力传感器感应到重量持续增加并发出信号,信号被控制器接收启动加热装置,使温度一直维持在75℃,当滴加完混合液后,信号消失,控制器控制加热装置关闭。
实施例3
一种耐高低温的弹性隔热板及其制备工艺,如图1所示,具体包括以下步骤:
S1:隔热基板的制作
S1.1:将3份硅酸铝纤维置于4份去离子水中,然后过80目筛制,使硅酸铝纤维中的渣球含量大幅降低,得硅酸铝纤维浆,将浓度为0.4%的硅酸铝纤维浆和浓度为0.6%的聚丙烯酰胺分散剂按3:2的比例混合,然后置于超声波乳化分散机进行超声分散8分钟,得到改性硅酸铝纤维,备用;
S1.2:将浓度为0.6%的聚丙烯酰胺、去离子水、铝溶胶、硅酸钙和改性硅酸铝纤维以1:2.5:0.2:1:4的质量比混合,硅酸钙、硅酸铝纤维均具备优秀的耐高低温性能,投入叶片式搅拌机中搅拌6分钟,再将所得混合液投入超声波乳化分散机,进行超声分散8分钟,使后续制备的硅酸钙/硅酸铝纤维复合材料获得更好的柔性,再投入循环水真空泵中真空抽滤12分钟,得到硅酸钙/硅酸铝纤维复合材料,备用;
S1.3:将1cm的垫片置于模压机底部,使压缩时隔热基板厚度控制在1cm,随后将硅酸钙/硅酸铝纤维复合材料投入模压机中以110℃压印15分钟,制得隔热基板,备用。
S2:PDMS预混粘结剂和溶剂型丙烯酸酯的制备
S2.1:将聚二甲基硅氧烷与固化剂按照10:1的质量比混合,随后置于烘干箱中以80℃的温度固化5分钟,然后将固化后的聚二甲基硅氧烷基体与硅酸钙颗粒和硅酸纤维以1:3:1.5的质量比进行混合,再将所得混合物投入非介入式材料均质机中,调节转速为2100rpm,均匀分散3分钟,制成PDMS预混粘结剂,备用;
S2.2:将2份丙烯酸丁酯、2份水溶性聚乙烯醇和0.25份丁烯二酸混合均匀,丙烯酸丁酯能够使粘结剂热合之后形成的膜具备优良的粘性,水溶性聚乙烯醇可以使粘结剂在热合时更好的形成薄膜,还能进一步增加膜的粘结能力并使成形的膜具有较低的热导率,丁烯二酸具有高透明度、耐热性和高稳定性等特点,在粘合剂中作为功能单体,可提高乳液的耐热性和稳定性,得到混合液,随后将3份蒸馏水和0.04份十二烷基苯磺酸钙盐加入容器中,容器加热至80℃,然后加入0.3份过硫酸铵、0.1份聚氧乙烯型非离子表面活性剂和0.2份混合液,静置15分钟后,向容器内缓慢滴加1.8份混合液,然后再加入0.2份过硫酸铵,容器持续加热使温度保持在80℃,静置30分钟,随后自然降温15分钟,使温度降至50℃,得到混合乳液,备用;
S2.3:将0.5份松香、0.05份烧碱和5份水装入三口烧瓶中,加热至100℃反应3小时,然后自然降温30分钟,使温度降至60℃,得到松香皂,将所得的1份松香皂加入4份乳液中混合搅拌20分钟,得到溶剂型丙烯酸酯,备用。
S3:间隔板的制备
S3.1:将4份固态硅酸钙置于容器中,再将坩埚置于高温电炉中,调节温度为1800℃熔融30分钟,随后加入粒径为2mm的增粘剂0.2份搅拌20分钟,然后加入0.01份发泡剂TiH2搅拌3分钟,对硅酸钙进行发泡处理,使硅酸钙能够获得高强度的压缩、弯曲能力,吸收更多的能量,具备良好的弹性,在1800℃温度下静置2分钟后将坩埚取出,将坩埚内的硅酸钙熔体倒入熔融造粒机中,调节制造粒径为1cm,直到硅酸钙熔体全部造粒完成,得到球形孔发泡硅酸钙球粒,球与球之间能实现较大转动,备用;
S3.2:将步骤S2.1中制得的PDMS预混粘结剂与发泡硅酸钙球粒以1:2的质量比混合,进一步增加材料的弹性,将所得混合物投入非介入式材料均质机,调节转速为2000rpm,均匀分散2分钟,再将均匀分散的混合物置入模压机中,调节温度为105℃,压缩15分钟,制得间隔板;
S3.3:将0.5份PDMS预混粘结剂均匀涂于隔热层的上下两面,随后置于模压机中,调节温度为110℃,压力为20Mpa,压缩15分钟,使隔热层上下两面生成封装层,进一步使间隔板的柔性与隔热性能得到提升,得到间隔板。
S4:制备反射复合膜
S4.1:将BOPP塑料薄膜装于真空蒸镀机中,再将纯度为99.9%以上的铝丝1份置于蒸镀机的坩埚中,启动真空泵使蒸镀机中的真空度达到1.3×10-2Pa,并启动加热器,使坩埚温度为1400℃,使铝丝气态化,控制BOPP塑料薄膜的移动速度为180m/分钟,并将铝丝镀在BOPP塑料薄膜表面,得到厚度为60nm的镀铝膜,随后打开冷却装置将镀铝膜冷却至60℃,然后取出自然冷却,得到镀铝膜成品;
S4.2:将1份溶剂型粘合剂丙烯酸酯均匀地涂在镀铝膜成品表面,使镀铝膜成品表面的上浆量为9g/m2,随后将其与两张6mm的PET膜置于覆膜机中,调节覆膜机烘道温度为60℃,加热辊的温度为120℃,加热辊卷绕线速度为6m/分钟,上卷张力为31.6N,经过2分钟,使镀铝膜成品两面均粘结上PET膜,覆膜机烘道首先对溶剂型粘合剂丙烯酸酯干燥除去溶剂,覆膜机再将表面干燥的镀铝膜成品送入加热辊,与PET膜相遇,镀铝膜与PET膜在热压状态下被粘合,得到反射复合膜,备用。
S5:隔热基板的覆膜与粘合
S5.1:将隔热基板一面均匀地涂上0.5份步骤S2.3制备的溶剂型丙烯酸酯,使用这种溶剂型丙烯酸酯粘结剂能够使隔热板各部分紧密结合,防止材料在发生形变时发生相对移动,使隔热板保持良好的弹性,同时还能够增强隔热板的隔热能力,使隔热基板一面的上浆量为9g/m2,将其与反射复合膜置入覆膜机中,调节覆膜机烘道温度为60℃,加热辊的温度为120℃,加热辊卷绕线速度为3m/分钟,上卷张力为33.7N,经过3分钟,得到覆膜隔热基板,备用;
S5.2:取两块覆膜隔热基板,均在未覆膜的一面均匀涂上0.5份步骤S2.1制备的PDMS预混粘结剂,将间隔板至于两块隔热基板之间,间隔板上下两面分别与覆膜隔热基板涂有PDMS预混粘结剂的一面接触,随后置于模压机中并启动模压机,调节模压机温度为110℃,压力为15Mpa,压缩15分钟,得到一种耐高低温的弹性隔热板,间隔板与同样具有良好的弹性的隔热基板粘合在一起,制得的隔热板具有更大的弹性,并且在获得更好的隔热能力的同时又不缺失强度。
S2.2的容器底部设有重力传感器,重力传感器可以控制容器底部的加热装置启动与关闭,当向容器中加入蒸馏水和十二烷基苯磺酸钙盐时,重力传感器感应到容器内重量增加发出信号,信号被加热装置上的控制器就接收从而启动加热装置,使容器温度达到80℃,再加入过硫酸铵、聚氧乙烯型非离子表面活性剂和混合液,重力传感器再次感应到容器内质量增加,使加热装置继续加热,容器温度达到80℃没有物质通过时,控制器控制加热装置停止加热,静置15分钟后,向容器内缓慢滴加混合液,重力传感器感应到重量持续增加并发出信号,信号被控制器接收启动加热装置,使温度一直维持在80℃,当滴加完混合液后,信号消失,控制器控制加热装置关闭。
与实施例1相比,对比例1的不同之处在于,对比例1为市售硅酸钙板,具体为莱州凯发隔热材料有限公司出售的硅酸钙板,记为对比例1。
将质量均为500g,形状为相同长方体,体积均为400cm3的实施例1、实施例2、实施例3制得的耐高低温的弹性隔热板和对比例1采用《GBT/10297-1998非金属固体材料导热系数测定方法》,在压强均为一个大气压,温度分别为-100℃,-75℃,20℃,75℃,150℃的环境下测试导热系数,不同温度的导热系数可以反应隔热板对高低温的耐受性,导热系数低则隔热效果好,则耐受性好,记录数据,将数据制成表格,参考图2,可以看出实施例1、实施例2、实施例3制得的耐高低温的弹性隔热板在低温和高温条件下导热系数与常温相差无几,而对比例1在低温条件下导热系数明显高于常温,在高温条件下相差无几,证明了实施例中的工艺流程能够得到一种耐高低温的隔热板。
上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。

Claims (9)

1.一种耐高低温的弹性隔热板的制备工艺,其特征在于,具体包括以下步骤:
S1:隔热基板的制作
将硅酸铝纤维进行超声分散之后与聚丙烯酰胺、去离子水、铝溶胶、硅酸钙混合搅拌,再对混合液进行超声分散,然后投入循环水真空泵中真空抽滤,得到硅酸钙/硅酸铝纤维复合材料,备用;
S2:PDMS预混粘结剂和溶剂型丙烯酸酯的制备
将聚二甲基硅氧烷与固化剂混合、干燥固化、均匀分散制得PDMS预混粘结剂,将丙烯酸丁酯、水溶性聚乙烯醇和丁烯二酸混合,得到混合液,将蒸馏水和十二烷基苯磺酸钙盐加入烧瓶加热,再加入混合液、过硫酸铵和非离子表面活性剂,持续加热反应,冷却后与松香皂混合得到溶剂型丙烯酸酯;
步骤S2中的松香皂由松香、烧碱和水混合加热之后冷却制得;
S3:间隔板的制备
将固态硅酸钙熔融,加入增粘剂搅拌,再加入发泡剂TiH2搅拌,将发泡的熔体加入熔融造粒机中造粒,得到球形孔发泡硅酸钙球粒,将球形孔发泡硅酸钙球粒与PDMS预混粘结剂混合、均匀分散、压缩,制得间隔板,备用;
S4:制备反射复合膜
将铝丝通过真空蒸镀机蒸镀在BOPP塑料薄膜上,得到镀铝膜成品,将溶剂型粘合剂丙烯酸酯涂在镀铝膜成品表面,在覆膜机中通过热合法使PET膜粘结在镀铝膜成品表面,得到反射复合膜,备用;
S5:隔热基板的覆膜与粘合
将隔热基板一面涂上溶剂型丙烯酸酯,在覆膜机中通过热合法使反射复合膜粘结在隔热基板涂有溶剂型丙烯酸酯的一面上,得到覆膜隔热基板,取两块覆膜隔热基板在未覆膜一面涂上PDMS预混粘结剂,将间隔板置于两块覆膜隔热基板之间,加热压缩,制得一种耐高低温的弹性隔热板。
2.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S1隔热基板的制作,具体包括以下步骤:
S1.1:将3-4份硅酸铝纤维置于4-5份去离子水中,然后过60-80目筛制得硅酸铝纤维浆,将浓度为0.4-0.6%的硅酸铝纤维浆和浓度为0.6-0.8%的聚丙烯酰胺分散剂按3:(2-2.5)的比例混合,然后置于超声波乳化分散机进行超声分散6-8分钟,得到改性硅酸铝纤维,备用;
S1.2:将浓度为0.6-0.8%的聚丙烯酰胺、去离子水、铝溶胶、硅酸钙和改性硅酸铝纤维以1:(2.5-3):(0.1-0.2):(0.5-1):(3-4)的质量比混合,投入叶片式搅拌机中搅拌5-6分钟,再将所得混合液投入超声波乳化分散机,进行超声分散6-8分钟,再投入循环水真空泵中真空抽滤10-12分钟,得到硅酸钙/硅酸铝纤维复合材料,备用;
S1.3:将1-1.5cm的垫片置于模压机底部,随后将硅酸钙/硅酸铝纤维复合材料投入模压机中以100-110℃压印10-15分钟,制得隔热基板,备用。
3.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S2PDMS预混粘结剂和溶剂型丙烯酸酯的制备,具体包括以下步骤:
S2.1:将聚二甲基硅氧烷与固化剂按照(10-15):1的质量比混合,随后置于烘干箱中以75-80℃的温度固化3-5分钟,然后将固化后的聚二甲基硅氧烷基体与硅酸钙颗粒和硅酸纤维以1:(3-3.5):(1.5-2)的质量比进行混合,再将所得混合物投入非介入式材料均质机中,调节转速为2000-2100rpm,均匀分散2-3分钟,制成PDMS预混粘结剂,备用;
S2.2:将2-3份丙烯酸丁酯、2-3份水溶性聚乙烯醇和0.25-0.3份丁烯二酸混合均匀,得到混合液,随后将3-5份蒸馏水和0.04-0.05份十二烷基苯磺酸钙盐加入容器中,容器加热至75-80℃,然后加入0.3-0.35份过硫酸铵、0.1-0.2份聚氧乙烯型非离子表面活性剂和0.2-0.3份混合液,静置10-15分钟后,向容器内缓慢滴加1.8-2.7份混合液,然后再加入0.2-0.3份过硫酸铵,容器持续加热使温度保持在75-80℃,静置25-30分钟,随后自然降温10-15分钟,使温度降至40-50℃,得到混合乳液,备用;
S2.3:将0.5-1份松香、0.05-0.1份烧碱和5-6份水装入三口烧瓶中,加热至80-120℃反应2-3小时,然后自然降温25-30分钟,使温度降至50-60℃,得到松香皂,将所得的1-2份松香皂加入4-5份乳液中混合搅拌15-20分钟,得到溶剂型丙烯酸酯,备用。
4.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S3间隔板的制备,具体包括以下步骤:
S3.1:将4-5份固态硅酸钙置于容器中,再将坩埚置于高温电炉中,调节温度为1600-1800℃熔融25-30分钟,随后加入粒径为2-3mm的增粘剂0.2-0.3份搅拌15-20分钟,然后加入0.01-0.04份发泡剂TiH2搅拌2-3分钟,在1600-1800℃温度下静置1-2分钟后将坩埚取出,将坩埚内的硅酸钙熔体倒入熔融造粒机中,调节制造粒径为1-1.5cm,直到硅酸钙熔体全部造粒完成,得到球形孔发泡硅酸钙球粒,备用;
S3.2:将步骤S2.1中制得的PDMS预混粘结剂与发泡硅酸钙球粒以1:(2-2.5)的质量比混合,将所得混合物投入非介入式材料均质机,调节转速为1900-2000rpm,均匀分散1-2分钟,再将均匀分散的混合物置入模压机中,调节温度为100-105℃,压缩10-15分钟,制得间隔板;
S3.3:将0.5-0.7份PDMS预混粘结剂均匀涂于隔热层的上下两面,随后置于模压机中,调节温度为100-110℃,压力为15-20Mpa,压缩10-15分钟,得到间隔板。
5.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S4制备反射复合膜,具体包括以下步骤:
S4.1:将BOPP塑料薄膜装于真空蒸镀机中,再将纯度为99.9%以上的铝丝1-1.5份置于蒸镀机的坩埚中,启动真空泵使蒸镀机中的真空度达到1.3×10-3~1.3×10-2Pa,并启动加热器,使坩埚温度为1200-1400℃,控制BOPP塑料薄膜的移动速度为170-180m/分钟,并将铝丝镀在BOPP塑料薄膜表面,得到厚度为60-70nm的镀铝膜,随后打开冷却装置将镀铝膜冷却至55-60℃,然后取出自然冷却,得到镀铝膜成品;
S4.2:将1-2份溶剂型粘合剂丙烯酸酯均匀地涂在镀铝膜成品表面,使镀铝膜成品表面的上浆量为9-12g/m2,随后将其与两张6-8mm的PET膜置于覆膜机中,调节覆膜机烘道温度为55-60℃,加热辊的温度为110-120℃,加热辊卷绕线速度为6-8m/分钟,上卷张力为29.4-31.6N,经过1-2分钟,使镀铝膜成品两面均粘结上PET膜,得到反射复合膜,备用。
6.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S5隔热基板的覆膜与粘合,具体包括以下步骤:
S5.1:将隔热基板一面均匀地涂上0.5-1份步骤S2.3制备的溶剂型丙烯酸酯,使隔热基板一面的上浆量为9-12g/m2,将其与反射复合膜置入覆膜机中,调节覆膜机烘道温度为55-60℃,加热辊的温度为110-120℃,加热辊卷绕线速度为3-5m/分钟,上卷张力为32.5-33.7N,经过2-3分钟,得到覆膜隔热基板,备用;
S5.2:取两块覆膜隔热基板,均在未覆膜的一面均匀涂上0.5-0.7份步骤S2.1制备的PDMS预混粘结剂,将间隔板至于两块隔热基板之间,间隔板上下两面分别与覆膜隔热基板涂有PDMS预混粘结剂的一面接触,随后置于模压机中并启动模压机,调节模压机温度为100-110℃,压力为10-15Mpa,压缩10-15分钟,得到一种耐高低温的弹性隔热板。
7.根据权利要求1所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S2.2的容器底部设有重力传感器,重力传感器可以控制容器底部的加热装置启动与关闭,当向容器中加入蒸馏水和十二烷基苯磺酸钙盐时,重力传感器感应到容器内重量增加发出信号,信号被加热装置上的控制器就接收从而启动加热装置,使容器温度达到75-80℃,再加入过硫酸铵、聚氧乙烯型非离子表面活性剂和混合液,重力传感器再次感应到容器内质量,使加热装置继续加热,容器温度达到75-80℃没有物质通过时,控制器控制加热装置停止加热,静置10-15分钟后,向容器内缓慢滴加混合液,重力传感器感应到物质持续通过并发出信号,信号被控制器接收启动加热装置,使温度一直维持在75-80℃,当滴加完混合液后,信号消失,控制器控制加热装置关闭。
8.根据权利要求5所述的一种耐高低温的弹性隔热板的制备工艺,其特征在于,步骤S3.1中的增粘剂为硅胶增粘剂。
9.一种耐高低温的弹性隔热板,其特征在于,其由上述权利要求1-8任一项的一种耐高低温的弹性隔热板的制备工艺得到。
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