CN111995791A - 一种热塑性轻型泡沫塑料的制备方法 - Google Patents
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Abstract
本发明公开了一种热塑性轻型泡沫塑料的制备方法,采用超临界CO2作为发泡剂对苯乙烯塑料进行发泡操作,配合加入纳米二氧化硅作为成核剂,可以有效降低泡孔直径,增加泡孔密度和均匀度,显著降低了PS发泡珠粒的容重。同时通过在阻燃液中加入容重极低,隔热性较好的SiO2气凝胶,有效降低了阻燃液的密度,在包覆阻燃液后,使泡沫塑料仍保持较低的容重,有效实现了阻燃泡沫材料的轻量化。
Description
技术领域
本发明涉及苯乙烯泡沫材料领域,特别涉及一种热塑性轻型泡沫塑料的制备方法。
背景技术
包覆阻燃是使用树脂、水、硅酸盐等能起到粘结作用的物质,与阻燃剂混合均匀,对EPS颗粒进行包覆处理,使阻燃剂牢固地吸附到发泡PS泡沫表面,进行模压成型从而实现阻燃。这种方法使可选择的阻燃剂种类更多,且阻燃剂的相容性、稳定性好,包覆物在颗粒外层己形成隔离防火层,因此阻燃性能更优,且为环保型阻燃剂阻燃PS泡沫板的应用提供了有利条件。包覆PS泡沫所用树脂常为热固性树脂,如:酚醛树脂、环氧树脂、三聚氰胺树脂或几种树脂的混合使用,外层树脂通常在固化剂或高温下交联固化,形成绝热防火层。其中,酚醛树脂除了能用做改善各种有机塑料和无机填料相容性的粘结剂,其本身有隔热性能良好、难燃、遇火炭化、离火自熄、低毒低烟等特点,是PS泡沫包覆溶剂的最佳选择。
连续挤出发泡的一般过程是将高压气体注入挤出机机筒后,达到熔融状态的聚合物通过螺杆的剪切混合作用,与注入的气体形成聚合物/气体的均相溶液。随后均相溶液进入熔体泵稳压输送,并在出口模前引发足够数量的气泡核,最后经定型流道流出模具。连续挤出发泡过程从设备,通过螺杆的输送和熔融,气源供给的气体通过计量泵连续稳定地输入挤出机中,通过双螺杆的混合剪切和静态混合器的充分混合,使气体充分溶解入聚合物熔体中,与熔融物料形成聚合物熔体/气体的均相溶液。然后通过快速降压(特殊喷嘴、熔体齿轮泵、快速释压元件等),使熔体压力快速下降,熔体中溶解的气体达到过饱和的不稳定状态,瞬间形成大量微小的气泡核。然后泡孔长大,含有大量气泡的熔体流入成型装置成型并在定型口模稳定和固化,得到发泡制塑料。
在发泡过程中,为了能形成大量气泡核,常采用加成核剂的方法,其目的是为了形成气泡核制造条件。成核剂的加入使均相成核变为非均相成核,成核剂使非均相熔体中存在大量的界面,可以大幅度降低所需要的成核势能,可以很好的改善成核情况。成核剂的种类很多,但有一点是相同的,都是使气体能聚集到此点形成气泡核。有的成核剂是粉状,加入聚合物熔体中形成的界面可成为成核点,也有发泡剂分解产生的热量,形成热点,成为成核点。也有加金属粉,通过材料间散热性能的差别,形成热点成核。常用的成核剂有滑石粉、碳酸钙、柠檬酸、金属粉等。
但PS发泡珠粒中成核剂、辅料的加入以及外包覆阻燃会显著增加泡沫材料的重量,影响轻量化,因此这一问题又待进一步解决。
发明内容
本发明所要解决的技术问题:在提高发泡质量及阻燃的同时有效降低泡沫塑料的容重。
为解决上述技术问题,本发明提供以下的技术方案:
一种热塑性轻型泡沫塑料的制备方法,具体步骤如下:
(a)将SiO2气凝胶粉末与质量分数90wt%的酚醛树脂混合,搅拌3-5min,搅拌速率大于100r/min,得阻燃液;
(b)将阻燃液与PS发泡珠粒混合,在电动搅拌机上500rpm,搅拌5min,使酚醛树脂包覆液均匀的涂覆在PS发泡珠粒表面,加入PS发泡珠粒20wt%的固化剂继续搅拌2min后取出得包覆发泡颗粒;
(c)将包覆发泡颗粒倒入模具中,将模具放置在平板硫化机中模压成型、陈化即得阻燃热塑性轻型泡沫材料。
优选地,所述硫化机上下板温度控制在103-105℃,成型压力8Mpa,时间4min。
优选地,所述阻燃液与PS发泡珠粒重量比为1:3。
优选地,所述SiO2气凝胶粉末与酚醛树脂的质量比为1:5~10。
优选地,所述PS发泡珠粒由如下方法制备获得:
(1)将苯乙烯与一定比例的纳米二氧化硅在高速搅拌机中混合均匀,在混合过程中加入苯乙烯重量3~7%的单甘脂/液体石蜡混合液,充分搅拌后得混合物一;
(2)将混合物一加入同向旋转双螺杆-单螺杆双阶挤出机中进行发泡,发泡过程中,向同向旋转双螺杆挤出机中注入超临界CO2,双螺杆挤出机各段温度分别为:174℃,182℃,187℃,184℃,178℃,178℃,179℃,175℃,175℃,螺杆转速为320rpm,注气量设定在0.8kg/h;
(3)随后由口模挤出得发泡坯料;
(4)将发泡坯料切碎成颗粒状,将坯料颗粒置于160℃恒温环境下,持续20min进行外封闭即得PS发泡珠粒。
优选地,所述纳米二氧化硅加入量为苯乙烯重量的5%,所述口模尺寸为:2mm×20mm,口模的温度为:113℃,所述超临界CO2的临界温度32℃,临界压力7.5Mpa。
本发明获得的有益效果:
采用超临界CO2作为发泡剂对苯乙烯塑料进行发泡操作,配合加入纳米二氧化硅作为成核剂,可以有效降低泡孔直径,增加泡孔密度和均匀度,显著降低了PS发泡珠粒的容重。同时通过在阻燃液中加入容重极低,隔热性较好的SiO2气凝胶,有效降低了阻燃液的密度,在包覆阻燃液后,使泡沫塑料仍保持较低的容重,有效实现了阻燃泡沫材料的轻量化。
具体实施方式
下面通过对实施例的描述,对本发明的具体实施方式作进一步详细的说明,以帮助本领域的技术人员对本发明的发明构思、技术方案有更完整、准确和深入的理解。
实施例1:按如下方法制备热塑性轻型泡沫塑料:
(1)将苯乙烯与苯乙烯重量5%的纳米二氧化硅在高速搅拌机中混合均匀,在混合过程中加入苯乙烯重量3%的单甘脂/液体石蜡混合液,充分搅拌后得混合物一;
(2)将混合物一加入同向旋转双螺杆-单螺杆双阶挤出机中,依次经过同向旋转双螺杆挤出机、单螺杆挤出机进行发泡,发泡过程中,向同向旋转双螺杆挤出机中注入超临界CO2,双螺杆挤出机各段温度分别为:174℃,182℃,187℃,184℃,178℃,178℃,179℃,175℃,175℃,螺杆转速为320rpm,注气量设定在0.8kg/h;同向双螺杆级出机:ZSK25-WLE型,螺杆长径比为40:1,直径为25mm。单螺杆挤出机:长径比20:1,直径45mm。
(3)随后由口模挤出得发泡坯料;口模尺寸为:2mm×20mm,口模的温度为:113℃,所述超临界CO2的临界温度32℃,临界压力7.5Mpa。
(4)将发泡坯料切碎成颗粒状,将坯料颗粒置于160℃恒温环境下,持续20min进行外封闭即得PS发泡珠粒。此步骤的目的在于封闭坯料颗粒表面外漏的泡孔,坯料颗粒的外壁在高温下粘合封闭,防止后续操作中液体渗入PS发泡珠粒中,影响包覆效果。
(5)按质量比为1:5将SiO2气凝胶粉末与质量分数90wt%的酚醛树脂混合,搅拌3min,搅拌速率大于100r/min,得阻燃液;
(6)按阻燃液与PS发泡珠粒重量比为1:3将二者混合,在电动搅拌机上500rpm,搅拌5min,使酚醛树脂包覆液均匀的涂覆在PS发泡珠粒表面,加入PS发泡珠粒20wt%的固化剂继续搅拌2min后取出得包覆发泡颗粒;
(7)将包覆发泡颗粒倒入模具中,将模具放置在平板硫化机中模压成型、陈化即得阻燃热塑性轻型泡沫材料。所述硫化机上下板温度控制在103-105℃,成型压力8Mpa,时间4min。
实施例2:按如下方法制备热塑性轻型泡沫塑料:
(1)将苯乙烯与苯乙烯重量5%的纳米二氧化硅在高速搅拌机中混合均匀,在混合过程中加入苯乙烯重量7%的单甘脂/液体石蜡混合液,充分搅拌后得混合物一;
(2)将混合物一加入同向旋转双螺杆-单螺杆双阶挤出机中,依次经过同向旋转双螺杆挤出机、单螺杆挤出机进行发泡,发泡过程中,向同向旋转双螺杆挤出机中注入超临界CO2,双螺杆挤出机各段温度分别为:174℃,182℃,187℃,184℃,178℃,178℃,179℃,175℃,175℃,螺杆转速为320rpm,注气量设定在0.8kg/h;同向双螺杆级出机:ZSK25-WLE型,螺杆长径比为40:1,直径为25mm。单螺杆挤出机:长径比20:1,直径45mm。
(3)随后由口模挤出得发泡坯料;口模尺寸为:2mm×20mm,口模的温度为:113℃,所述超临界CO2的临界温度32℃,临界压力7.5Mpa。
(4)将发泡坯料切碎成颗粒状,将坯料颗粒置于160℃恒温环境下,持续20min进行外封闭即得PS发泡珠粒。
(5)按质量比为1:10将SiO2气凝胶粉末与质量分数90wt%的酚醛树脂混合,搅拌5min,搅拌速率大于100r/min,得阻燃液;
(6)按阻燃液与PS发泡珠粒重量比为1:3将二者混合,在电动搅拌机上500rpm,搅拌5min,使酚醛树脂包覆液均匀的涂覆在PS发泡珠粒表面,加入PS发泡珠粒20wt%的固化剂继续搅拌2min后取出得包覆发泡颗粒;
(7)将包覆发泡颗粒倒入模具中,将模具放置在平板硫化机中模压成型、陈化即得阻燃热塑性轻型泡沫材料。所述硫化机上下板温度控制在103-105℃,成型压力8Mpa,时间4min。
实施例3:按如下方法制备热塑性轻型泡沫塑料:
(1)将苯乙烯与苯乙烯重量5%的纳米二氧化硅在高速搅拌机中混合均匀,在混合过程中加入苯乙烯重量5%的单甘脂/液体石蜡混合液,充分搅拌后得混合物一;
(2)将混合物一加入同向旋转双螺杆-单螺杆双阶挤出机中,依次经过同向旋转双螺杆挤出机、单螺杆挤出机进行发泡,发泡过程中,向同向旋转双螺杆挤出机中注入超临界CO2,双螺杆挤出机各段温度分别为:174℃,182℃,187℃,184℃,178℃,178℃,179℃,175℃,175℃,螺杆转速为320rpm,注气量设定在0.8kg/h;同向双螺杆级出机:ZSK25-WLE型,螺杆长径比为40:1,直径为25mm。单螺杆挤出机:长径比20:1,直径45mm。
(3)随后由口模挤出得发泡坯料;口模尺寸为:2mm×20mm,口模的温度为:113℃,所述超临界CO2的临界温度32℃,临界压力7.5Mpa。
(4)将发泡坯料切碎成颗粒状,将坯料颗粒置于160℃恒温环境下,持续20min进行外封闭即得PS发泡珠粒。
(5)按质量比为1:8将SiO2气凝胶粉末与质量分数90wt%的酚醛树脂混合,搅拌4min,搅拌速率大于100r/min,得阻燃液;
(6)按阻燃液与PS发泡珠粒重量比为1:3将二者混合,在电动搅拌机上500rpm,搅拌5min,使酚醛树脂包覆液均匀的涂覆在PS发泡珠粒表面,加入PS发泡珠粒20wt%的固化剂继续搅拌2min后取出得包覆发泡颗粒;
(7)将包覆发泡颗粒倒入模具中,将模具放置在平板硫化机中模压成型、陈化即得阻燃热塑性轻型泡沫材料。所述硫化机上下板温度控制在103-105℃,成型压力8Mpa,时间4min。
对照实施例1:其余均与实施例3相同,不同之处在于将SiO2气凝胶粉末替换为等粒径的SiO2粉末。
对照实施例2:其余均与实施例3相同,不同之处在于采用等重的纯EPS发泡颗粒替换PS发泡珠粒。
将实施例1~3及对照实施例1~2制备的泡沫塑料分别测定采用HC-2C型氧指数测定仪测定泡沫材料的极限氧指数(LOI)和容重,首先按照国标GB 2408-80要求,制样为长80-150mm,宽10±0.5mm,厚10±0.5mm的长方体泡沫材料,调整氮氧比例,测定材料的极限氧指数值。结果见表1:
表1不同阻燃材料的极限氧指数值
组别 | LOI(%) | 容重(g/L) |
实施例1 | 27.0 | 23.4 |
实施例2 | 28.0 | 25.3 |
实施例3 | 27.0 | 22.6 |
对照实施例1 | 23.5 | 35.7 |
对照实施例2 | 28.5 | 27.7 |
LOI值是评价塑料制品燃烧行为的常用标准,LOI值的大小表示物体在燃烧过程中的难易程度,LOI值越大大,表示该物体难燃烧;LOI值越小,表示该物体易于燃烧,阻燃性能差。LOI值低于22时为易燃物,22~27为可燃物,27以上为难燃物。
采用类似于粉末二氧化硅的无机阻燃剂掺入酚醛树脂中后,在本发明公开的重量配比下,阻燃层密度增大,体积缩小,导致包覆阻燃层变薄,显著降低了泡沫材料的阻燃性能,也降低了材料的整体容重。
采用本申请中超临界二氧化碳及纳米二氧化硅制备的发泡塑料在容重上低于传统的EPS发泡颗粒,但省去了聚合、浸渍、预发泡、熟化等诸多步骤,有效实现了PS泡沫塑料的轻量化。
泡孔结构是从微观角度对PS泡沫制品进行分析,包括平均泡孔直径和泡孔密度两项指标,是衡量制品发泡质量的重要指标。采用电镜扫描样本断面统计平均泡孔直径和泡孔密度,结果见表2:
表2不同发泡塑料的泡孔结构测定结果
表2结果表明本申请中的PS发泡颗粒制备工艺可以有效减小平均泡孔直径,提高泡孔密度,使得发泡颗粒内充满均匀细密的气泡,相比EPS发泡颗粒中的粗大泡孔,可以有效提高泡沫塑料成品的机械强度和韧性,且没有热胀冷缩现象,无需熟化步骤,
综上所述,采用超临界CO2作为发泡剂对苯乙烯塑料进行发泡操作,配合加入纳米二氧化硅作为成核剂,可以有效降低泡孔直径,增加泡孔密度和均匀度,显著降低了PS发泡珠粒的容重。同时通过在阻燃液中加入容重极低,隔热性较好的SiO2气凝胶,有效降低了阻燃液的密度,在包覆阻燃液后,使泡沫塑料仍保持较低的容重,有效实现了阻燃泡沫材料的轻量化。
以上实施例仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明保护范围之内;本发明未涉及的技术均可通过现有技术加以实现。
Claims (6)
1.一种热塑性轻型泡沫塑料的制备方法,其特征在于,具体步骤如下:
(a)将SiO2气凝胶粉末与质量分数90wt%的酚醛树脂混合,搅拌3-5min,搅拌速率大于100r/min,得阻燃液;
(b)将阻燃液与PS发泡珠粒混合,在电动搅拌机上500rpm,搅拌5min,使酚醛树脂包覆液均匀的涂覆在PS发泡珠粒表面,加入PS发泡珠粒20wt%的固化剂继续搅拌2min后取出得包覆发泡颗粒;
(c)将包覆发泡颗粒倒入模具中,将模具放置在平板硫化机中模压成型、陈化即得阻燃热塑性轻型泡沫材料。
2.根据权利要求1中所述的一种热塑性轻型泡沫塑料的制备方法,其特征在于:所述硫化机上下板温度控制在103-105℃,成型压力8Mpa,时间4min。
3.根据权利要求1中所述的一种热塑性轻型泡沫塑料的制备方法,其特征在于:所述阻燃液与PS发泡珠粒重量比为1:3。
4.根据权利要求1中所述的一种热塑性轻型泡沫塑料的制备方法,其特征在于:所述SiO2气凝胶粉末与酚醛树脂的质量比为1:5~10。
5.根据权利要求1中所述的一种热塑性轻型泡沫塑料的制备方法,其特征在于:所述PS发泡珠粒由如下方法制备获得:
(1)将苯乙烯与一定比例的纳米二氧化硅在高速搅拌机中混合均匀,在混合过程中加入苯乙烯重量3~7%的单甘脂/液体石蜡混合液,充分搅拌后得混合物一;
(2)将混合物一加入同向旋转双螺杆-单螺杆双阶挤出机中进行发泡,发泡过程中,向同向旋转双螺杆挤出机中注入超临界CO2,双螺杆挤出机各段温度分别为:174℃,182℃,187℃,184℃,178℃,178℃,179℃,175℃,175℃,螺杆转速为320rpm,注气量设定在0.8kg/h;
(3)随后由口模挤出得发泡坯料;
(4)将发泡坯料切碎成颗粒状,将坯料颗粒置于160℃恒温环境下,持续20min进行外封闭即得PS发泡珠粒。
6.根据权利要求5中所述的一种热塑性轻型泡沫塑料的制备方法的制备方法,其特征在于:所述纳米二氧化硅加入量为苯乙烯重量的5%,所述口模尺寸为:2mm×20mm,口模的温度为:113℃,所述超临界CO2的临界温度32℃,临界压力7.5Mpa。
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