CN114854194A - 一种阻燃塑料母粒及其制备方法 - Google Patents
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Abstract
本发明公开了一种阻燃塑料母粒及其制备方法,属于功能塑料技术领域,按质量份计,包括如下组分:尼龙66片材200份、碳纤维粉15‑18份、增容剂20份、聚四氟乙烯5‑9份、白炭黑5‑8份和阻燃颗粒35‑40份;该阻燃塑料母粒在制备过程中共进行两次熔融挤出,首先将尼龙66片材与碳纤维粉、增容剂、聚四氟乙烯和白炭黑熔融挤出,增容剂中含有不饱和的双键,有利于减小无机原料和有机原料间的界面差别,可以提高各原料之间的相容性;第二次熔融挤出时,尼龙66末端的羧基和氨基和聚乳酸末端的羟基和羧基发生共聚反应,进一步提高各组分之间的相容性,提高该阻燃塑料母粒的产品稳定性。
Description
技术领域
本发明属于功能塑料技术领域,具体涉及一种阻燃塑料母粒及其制备方法。
背景技术
聚酰胺俗称尼龙,是一种应用广泛的工程塑料,具有耐磨损、抗冲击、耐疲劳、耐油、耐腐蚀等优点。聚己二酰己二胺又叫尼龙66,是工程塑料中较为常用的一种,一般由己二酸和己二胺缩聚而成,不溶于一般溶剂,仅溶于间苯甲酚等。尼龙66具有较高的机械强度和硬度,刚性很大,可以制作齿轮、润滑轴承等机械附件,还可以代替有色金属制作机器外壳和发动机叶片等。
一些阻燃剂与聚合物之间的相容性不好,不能直接进行共混改性,否则会降低其使用强度,所以需要增加阻燃剂和尼龙66之间的相容性,满足阻燃要求的同时改善制备出的塑料制品的性能。
发明内容
本发明的目的在于提供一种阻燃塑料母粒及其制备方法,以解决背景技术中的问题。
本发明的目的可以通过以下技术方案实现:
一种阻燃塑料母粒,按质量份计,包括如下组分:尼龙66片材200份、碳纤维粉15-18份、增容剂20份、聚四氟乙烯5-9份、白炭黑5-8份和阻燃颗粒35-40份。
进一步地,增容剂通过如下步骤制备:
步骤S1:向烧瓶中加入去离子水、乳化剂,在300-400r/min的条件下搅拌均匀,然后向烧瓶中加入十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷、六甲基二硅氧烷,回流反应3-5h;十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷在酸性的条件下发生开环,然后与六甲基二硅氧烷发生聚合反应,得到侧链带有双键的中间产物1;冷却后得到含有中间产物1的乳液。
反应过程如下所示:
步骤S2:将含有中间产物1的乳液升温至80-90℃,在氮气保护和300-400r/min的条件下搅拌,向烧瓶中加入质量分数为3%的氢氧化钠溶液,调节乳液的pH值为7-8,向烧瓶中加入苯乙烯,然后滴加质量分数为15%的过硫酸铵溶液,继续反应4-5h;向烧瓶中加入甲基丙烯酸羟乙酯,然后滴加与上一次同量的质量分数为15%的过硫酸铵溶液,继续反应4-5h;过硫酸铵为引发剂,中间产物1、苯乙烯和甲基丙烯酸羟乙酯中的碳碳双键发生聚合反应,形成共聚物从而得到共聚物乳液;冷却后向烧瓶中加入混合溶剂与共聚物乳液一起搅拌20-30min,将共聚物乳液破乳,用索氏抽提器抽滤以便除去未反应的各种单体及均聚物,然后将剩余的共聚物用蒸馏水洗涤3-5次,在60℃的条件下真空干燥,得到白色粉末状的增容剂。
反应过程如下所示:
进一步地,乳化剂为十二烷基苯磺酸和辛基苯酚聚氧乙烯醚按照3:1的质量比混合制得。
进一步地,步骤S1中去离子水、乳化剂、十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷、六甲基二硅氧烷的用量比为150mL:25-30mL:37mL:45mL:25mL。
进一步地,步骤S2中含有中间产物1的乳液、苯乙烯、甲基丙烯酸羟乙酯、过硫酸铵溶液的用量比为200mL:80mL:80mL:25mL。
进一步地,混合溶剂为甲醇和丙酮按照1:1的质量比混合制得。
进一步地,阻燃颗粒通过如下步骤制备:将氢氧化镁和硅烷偶联剂加入烧瓶中,使硅烷偶联剂浸没氢氧化镁,在300-400r/min的条件下搅拌30-40min,然后抽滤取固体并在60℃的条件下干燥,得到改性氢氧化镁;将改性氢氧化镁、膨胀型阻燃剂和聚乳酸加入捏合机中捏合,然后挤出切成1-1.5cm的颗粒,得到阻燃颗粒。
进一步地,改性氢氧化镁、膨胀型阻燃剂和聚乳酸的用量比为20g:13-15g:50g;其中膨胀型阻燃剂购买于南京中宸新材料有限公司。
一种阻燃塑料母粒的制备方法为:将尼龙66片材、碳纤维粉、增容剂、聚四氟乙烯和白炭黑加入捏合机中,在190-220℃的条件下捏合20-30min,用双螺杆挤出机挤出并切成长度为1-1.5cm的颗粒,然后和阻燃颗粒混合,用捏合机在200-250℃的条件下捏合20-30min,最后用双螺杆挤出并切粒,得到阻燃塑料母粒。
本发明的有益效果:
该阻燃塑料母粒在制备过程中共进行两次熔融挤出,首先将尼龙66片材与碳纤维粉、增容剂、聚四氟乙烯和白炭黑熔融挤出,碳纤维粉可以增加制备出的塑料母粒的强度,增容剂中含有不饱和的双键,有利于减小无机原料和有机原料间的界面差别,具有很好的增容作用,便于提高各原料之间的相容性;聚四氟乙烯的摩擦系数极低,作为分散剂便于各组分在捏合时分散均匀,白炭黑可以增加其韧性;第二次熔融挤出时,阻燃颗粒中的聚乳酸呈微球状均匀地分散在尼龙66构成的基体中,形成类似于海岛的结构,并且聚乳酸和尼龙66在熔融加工过程中,尼龙66末端的羧基和氨基和聚乳酸末端的羟基和羧基发生共聚反应,使聚乳酸和尼龙66间又有较高的界面粘结力和良好的相容性,进一步提高各组分之间的相容性,提高该阻燃塑料母粒的产品稳定性。
阻燃颗粒中氢氧化镁经过硅烷偶联剂进行处理,增加了氢氧化镁的分散性,与膨胀型阻燃剂协同增加塑料母粒的阻燃性能,与聚乳酸捏合后再通过后续步骤与尼龙66熔融挤出,有利于这两种阻燃成分与其他材料混匀,并且增容剂原料中的各单体均具有较好的耐热性,使制备出的增容剂也具有较好的耐热性,与其余阻燃成分协同提高阻燃效果。
具体实施方式
下面将结合本发明实施例,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
制备增容剂,包括如下步骤:
步骤S1:将十二烷基苯磺酸和辛基苯酚聚氧乙烯醚按照3:1的质量比混合得到乳化剂;向烧瓶中加入150mL去离子水、25mL乳化剂,在300r/min的条件下搅拌均匀,然后向烧瓶中加入37mL十甲基环五硅氧烷、45mL五甲基五乙烯基环五硅氧烷和25mL六甲基二硅氧烷,回流反应3h;十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷在酸性的条件下发生开环,然后与六甲基二硅氧烷发生聚合反应,得到侧链带有双键的中间产物1;冷却后得到含有中间产物1的乳液。
步骤S2:将甲醇和丙酮按照1:1的质量比混合得到混合溶剂;将200mL含有中间产物1的乳液升温至80℃,在氮气保护和300r/min的条件下搅拌,向烧瓶中加入质量分数为3%的氢氧化钠溶液,调节乳液的pH值为7-8,向烧瓶中加入80mL苯乙烯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应4h;向烧瓶中加入80mL甲基丙烯酸羟乙酯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应4h;过硫酸铵为引发剂,中间产物1、苯乙烯和甲基丙烯酸羟乙酯中的碳碳双键发生聚合反应,形成共聚物从而得到共聚物乳液;冷却后向烧瓶中加入混合溶剂与共聚物乳液一起搅拌20min,将共聚物乳液破乳,用索氏抽提器抽滤以便除去未反应的各种单体及均聚物,然后将剩余的共聚物用蒸馏水洗涤3次,在60℃的条件下真空干燥,得到白色粉末状的增容剂。
实施例2
制备增容剂,包括如下步骤:
步骤S1:将十二烷基苯磺酸和辛基苯酚聚氧乙烯醚按照3:1的质量比混合得到乳化剂;向烧瓶中加入150mL去离子水、28mL乳化剂,在350r/min的条件下搅拌均匀,然后向烧瓶中加入37mL十甲基环五硅氧烷、45mL五甲基五乙烯基环五硅氧烷和25mL六甲基二硅氧烷,回流反应4h;十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷在酸性的条件下发生开环,然后与六甲基二硅氧烷发生聚合反应,得到侧链带有双键的中间产物1;冷却后得到含有中间产物1的乳液。
步骤S2:将甲醇和丙酮按照1:1的质量比混合得到混合溶剂;将200mL含有中间产物1的乳液升温至85℃,在氮气保护和350r/min的条件下搅拌,向烧瓶中加入质量分数为3%的氢氧化钠溶液,调节乳液的pH值为7.5,向烧瓶中加入80mL苯乙烯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应4.5h;向烧瓶中加入80mL甲基丙烯酸羟乙酯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应4.5h;过硫酸铵为引发剂,中间产物1、苯乙烯和甲基丙烯酸羟乙酯中的碳碳双键发生聚合反应,形成共聚物从而得到共聚物乳液;冷却后向烧瓶中加入混合溶剂与共聚物乳液一起搅拌25min,将共聚物乳液破乳,用索氏抽提器抽滤以便除去未反应的各种单体及均聚物,然后将剩余的共聚物用蒸馏水洗涤4次,在60℃的条件下真空干燥,得到白色粉末状的增容剂。
实施例3
制备增容剂,包括如下步骤:
步骤S1:将十二烷基苯磺酸和辛基苯酚聚氧乙烯醚按照3:1的质量比混合得到乳化剂;向烧瓶中加入150mL去离子水、30mL乳化剂,在400r/min的条件下搅拌均匀,然后向烧瓶中加入37mL十甲基环五硅氧烷、45mL五甲基五乙烯基环五硅氧烷和25mL六甲基二硅氧烷,回流反应5h;十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷在酸性的条件下发生开环,然后与六甲基二硅氧烷发生聚合反应,得到侧链带有双键的中间产物1;冷却后得到含有中间产物1的乳液。
步骤S2:将甲醇和丙酮按照1:1的质量比混合得到混合溶剂;将200mL含有中间产物1的乳液升温至90℃,在氮气保护和400r/min的条件下搅拌,向烧瓶中加入质量分数为3%的氢氧化钠溶液,调节乳液的pH值为8,向烧瓶中加入80mL苯乙烯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应5h;向烧瓶中加入80mL甲基丙烯酸羟乙酯,然后滴加12.5mL质量分数为15%的过硫酸铵溶液,继续反应5h;过硫酸铵为引发剂,中间产物1、苯乙烯和甲基丙烯酸羟乙酯中的碳碳双键发生聚合反应,形成共聚物从而得到共聚物乳液;冷却后向烧瓶中加入混合溶剂与共聚物乳液一起搅拌30min,将共聚物乳液破乳,用索氏抽提器抽滤以便除去未反应的各种单体及均聚物,然后将剩余的共聚物用蒸馏水洗涤5次,在60℃的条件下真空干燥,得到白色粉末状的增容剂。
实施例4
制备阻燃颗粒,包括如下步骤:
将氢氧化镁和硅烷偶联剂加入烧瓶中,使硅烷偶联剂浸没氢氧化镁,在300r/min的条件下搅拌30min,然后抽滤取固体并在60℃的条件下干燥,得到改性氢氧化镁;将20g改性氢氧化镁、13g膨胀型阻燃剂和50g聚乳酸加入捏合机中捏合,然后挤出切成1cm的颗粒,得到阻燃颗粒。
实施例5
制备阻燃颗粒,包括如下步骤:
将氢氧化镁和硅烷偶联剂加入烧瓶中,使硅烷偶联剂浸没氢氧化镁,在350r/min的条件下搅拌35min,然后抽滤取固体并在60℃的条件下干燥,得到改性氢氧化镁;将20g改性氢氧化镁、14g膨胀型阻燃剂和50g聚乳酸加入捏合机中捏合,然后挤出切成1.2cm的颗粒,得到阻燃颗粒。
实施例6
制备阻燃颗粒,包括如下步骤:
将氢氧化镁和硅烷偶联剂加入烧瓶中,使硅烷偶联剂浸没氢氧化镁,在400r/min的条件下搅拌40min,然后抽滤取固体并在60℃的条件下干燥,得到改性氢氧化镁;将20g改性氢氧化镁、15g膨胀型阻燃剂和50g聚乳酸加入捏合机中捏合,然后挤出切成1.5cm的颗粒,得到阻燃颗粒。
实施例7
制备阻燃塑料母粒,包括如下步骤:
将200g尼龙66片材、15g碳纤维粉、20g实施例1中制得的增容剂、5g聚四氟乙烯和5g白炭黑加入捏合机中,在190℃的条件下捏合20min,用双螺杆挤出机挤出并切成长度为1cm的颗粒,然后和35g实施例4中制得的阻燃颗粒混合,用捏合机在200℃的条件下捏合20min,最后用双螺杆挤出并切粒,得到阻燃塑料母粒。
实施例8
制备阻燃塑料母粒,包括如下步骤:
将200g尼龙66片材、16g碳纤维粉、20g实施例2中制得的增容剂、7g聚四氟乙烯和6g白炭黑加入捏合机中,在200℃的条件下捏合25min,用双螺杆挤出机挤出并切成长度为1.2cm的颗粒,然后和38g实施例5中制得的阻燃颗粒混合,用捏合机在230℃的条件下捏合25min,最后用双螺杆挤出并切粒,得到阻燃塑料母粒。
实施例9
制备阻燃塑料母粒,包括如下步骤:
将200g尼龙66片材、18g碳纤维粉、20g实施例3中制得的增容剂、9g聚四氟乙烯和8g白炭黑加入捏合机中,在220℃的条件下捏合30min,用双螺杆挤出机挤出并切成长度为1.5cm的颗粒,然后和40g实施例6中制得的阻燃颗粒混合,用捏合机在250℃的条件下捏合30min,最后用双螺杆挤出并切粒,得到阻燃塑料母粒。
对比例1:在实施例9的基础上,不添加增容剂,其余步骤保持不变,制备出塑料母粒。
对比例2:在实施例9的基础上,不添加阻燃颗粒,其余步骤保持不变,制备出塑料母粒。
对实施例7-实施例9、对比例1和对比例2进行性能测试,将各组制得的塑料母粒注塑成长度为15cm,宽1cm和厚度为4mm的试样条,并将各试样条根据GB/T 1040.1-2018测试其拉伸强度,根据GB/T 1043.1-2008测试其悬臂梁缺口冲击强度,并按照MT 113-1995进行酒精喷灯试验,结果如表1所示:
表1
由表1可以看出,实施例7-实施例9中的塑料母粒制得的试样条具有较好的拉伸强度和阻燃效果。
需要说明的是,在本文中,诸如术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (8)
1.一种阻燃塑料母粒,其特征在于,按质量份计,包括以下原料:尼龙66片材200份、碳纤维粉15-18份、增容剂20份、聚四氟乙烯5-9份、白炭黑5-8份和阻燃颗粒35-40份;
其中增容剂通过如下步骤制备:
步骤S1:向烧瓶中加入去离子水、乳化剂,在300-400r/min的条件下搅拌均匀,然后向烧瓶中加入十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷、六甲基二硅氧烷,回流反应3-5h,冷却后得到含有中间产物1的乳液;
步骤S2:将含有中间产物1的乳液升温至80-90℃,在氮气保护和300-400r/min的条件下搅拌,向烧瓶中加入氢氧化钠溶液调节乳液的pH值为7-8,向烧瓶中加入苯乙烯,然后滴加过硫酸铵溶液反应4-5h;向烧瓶中加入甲基丙烯酸羟乙酯,然后滴加与上一次同量的过硫酸铵溶液反应4-5h,反应后进行后处理得到白色粉末状的增容剂。
2.根据权利要求1所述的一种阻燃塑料母粒,其特征在于,步骤S2中后处理方法为:将反应体系冷却后加入混合溶剂搅拌20-30min,抽滤除去未反应的单体及均聚物,将剩余的共聚物用蒸馏水洗涤3-5次,在60℃的条件下真空干燥。
3.根据权利要求1所述的一种阻燃塑料母粒,其特征在于,乳化剂为十二烷基苯磺酸和辛基苯酚聚氧乙烯醚按照3:1的质量比混合制得。
4.根据权利要求1所述的一种阻燃塑料母粒,其特征在于,步骤S1中去离子水、乳化剂、十甲基环五硅氧烷、五甲基五乙烯基环五硅氧烷、六甲基二硅氧烷的用量比为150mL:25-30mL:37mL:45mL:25mL。
5.根据权利要求1所述的一种阻燃塑料母粒,其特征在于,步骤S2中含有中间产物1的乳液、苯乙烯、甲基丙烯酸羟乙酯、过硫酸铵溶液的用量比为200mL:80mL:80mL:25mL。
6.根据权利要求1所述的一种阻燃塑料母粒,其特征在于,阻燃颗粒的制备方法为:将氢氧化镁和硅烷偶联剂加入烧瓶中,使硅烷偶联剂浸没氢氧化镁,在300-400r/min的条件下搅拌30-40min,然后抽滤取固体并在60℃的条件下干燥,得到改性氢氧化镁;将改性氢氧化镁、膨胀型阻燃剂和聚乳酸加入捏合机中捏合,然后挤出切成1-1.5cm的颗粒,得到阻燃颗粒。
7.根据权利要求6所述的一种阻燃塑料母粒,其特征在于,改性氢氧化镁、膨胀型阻燃剂和聚乳酸的用量比为20g:13-15g:50g。
8.根据权利要求1所述的一种阻燃塑料母粒的制备方法,其特征在于,包括如下步骤:
将尼龙66片材、碳纤维粉、增容剂、聚四氟乙烯和白炭黑加入捏合机中,在190-220℃的条件下捏合20-30min,用双螺杆挤出机挤出并切成长度为1-1.5cm的颗粒,然后和阻燃颗粒混合,用捏合机在200-250℃的条件下捏合20-30min,最后用双螺杆挤出并切粒,得到阻燃塑料母粒。
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