CN106589656A - 一种阻燃母粒及其制备得到的阻燃型pvc木塑墙板 - Google Patents

一种阻燃母粒及其制备得到的阻燃型pvc木塑墙板 Download PDF

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CN106589656A
CN106589656A CN201610889715.6A CN201610889715A CN106589656A CN 106589656 A CN106589656 A CN 106589656A CN 201610889715 A CN201610889715 A CN 201610889715A CN 106589656 A CN106589656 A CN 106589656A
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Abstract

本发明属于环保木塑材料技术领域，具体公开了一种阻燃母粒，包括如下按重量份数计的组分制成：PVC树脂40~70；八钼酸铵0~30；改性氢氧化镁5~30；改性炭黑5~30；改性聚磷酸铵5~30；所述改性氢氧化镁采用表面活性剂和分散剂与氯化镁反应后获得；所述改性炭黑采用偶联剂A和炭黑反应获得；所述改性聚磷酸铵采用偶联剂B与聚磷酸铵反应后所得；本发明提供的阻燃母粒应用于制备木塑复合材料，能够获得较好的阻燃效果，产品防火性能好，燃烧过程黑烟和有毒害气体释放量小，提升了安全性能，应用前景好。

Description

一种阻燃母粒及其制备得到的阻燃型PVC木塑墙板
技术领域
本发明属于环保木塑材料技术领域，更具体地，涉及一种阻燃母粒及其制备得到的阻燃型PVC木塑墙板。
背景技术
由于木塑中的植物纤维和塑料均属于易燃材料，自身不具备阻燃性能，故存在着火灾等安全隐患，限制了现有的木塑复合材料的应用。为此，对木塑阻燃性能的研究一直受到人们的重视，
另一方面，现有的以聚氯乙烯树脂作为基体制备得到的木塑复合材料，其在燃烧过程中难以软化，有黑烟产生，并有刺激性酸味产生，同时还会释放出盐酸和氯气等有毒气体。当前对PVC阻燃抑烟的途径主要分为以下两种：一是使烟尘微粒氧化为气体CO和CO2；二是通过抑制其热分解产生的苯及其衍生物，从而促进残余炭的生成。目前PVC阻燃抑烟剂按组分的不同可分为三种，即无机阻燃抑烟剂、有机阻燃抑烟剂和复合(有机、无机混合)阻燃抑烟剂，而任何一种阻燃抑烟剂自身都有一些缺陷，故需研究阻燃抑烟剂的复配技术，发挥阻燃抑烟剂的协同作用，不但可以增强阻燃抑烟效果，提高加工性能和物理性能，而且还可以减小用量、降低成本及对环境的危害。
发明内容
本发明的目的在于根据现有技术中的不足，提供了一种阻燃母粒及其制备得到的阻燃型PVC木塑墙板。
本发明的目的通过以下技术方案实现：
本发明先经沉淀法以及湿法改性法制备(针状)改性氢氧化镁，然后采用表面改性法将炭黑经过钛酸酯偶联剂101(DN-101)表面改性得到改性炭黑，再用KH550对聚磷酸铵(APP)进行表面修饰得到改性聚磷酸铵(M-APP)，最后将八钼酸铵、(针状)改性氢氧化镁、改性炭黑、M-APP及PVC树脂进行熔融共混挤出得到新型阻燃母粒。
本发明提供了一种阻燃母粒，包括如下按重量份数计的组分制成：
所述改性氢氧化镁采用表面活性剂和分散剂与氯化镁反应后获得；
所述改性炭黑采用偶联剂A和炭黑反应获得；
所述改性聚磷酸铵采用偶联剂B与聚磷酸铵反应后所得。
本发明将氢氧化镁进行改性，能够提高其在聚合物基体中的相容性和分散性，聚磷酸铵改性能够提高其疏水性和在聚合物基体中的相容性，炭黑作为一种惰性填料，经过改性之后，填充到阻燃母粒中，可以提高氧指数，从而提高产品的阻燃性能。
优选地，所述偶联剂A为γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、N,N'＝双(2-甲基-2-硝基两基)-1.6-二氨基己烷、异丙基二油酸酰氧基钛酸酯或双-[γ-(三乙氧基硅)丙基]四硫化物，所述偶联剂B为有机硅偶联剂、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、γ―氨丙基三乙氧基硅烷或焦磷酸型单烷氧基钛酸酯。
优选地，将氯化镁溶液滴加到含有表面活性剂和分散剂的NaOH溶液中，滴加完后陈化一定时间，水浴加热，过滤洗涤，干燥即得改性氢氧化镁，表面活性剂和分散剂的添加总量占改性氢氧化镁生成量的2.5～3.5％。
优选地，所述表面活性剂为硬脂酸钠或十二烷基苯磺酸钠，所述分散剂为聚乙二醇1000。
优选地，偶联剂A加入到乙醇中，加入炭黑，超声，水浴加热，离心，洗涤，干燥后即得所述改性炭黑，偶联剂A与炭黑的混合质量比为1：(1～3)。
优选地，偶联剂A为钛酸酯偶联剂101。
优选地，将偶联剂B加入到乙醇中，加入聚磷酸铵，超声，水浴加热，离心，洗涤，干燥后即得所述改性聚磷酸铵，偶联剂B与聚磷酸铵的混合固液比为1：(40～60)。
优选地，偶联剂B为KH550。本发明同时提供一种阻燃型PVC木塑墙板，包括所述的阻燃母粒。
优选地，所述阻燃型PVC木塑墙板包括如下按重量份数计的组分制成：
在不影响本发明木塑墙板的性能前提下，其他助剂的添加同样在本发明阻燃型PVC木塑墙板保护范围之内，例如，发泡助剂，稳定剂或润滑剂等等。
与现有技术相比，本发明具有以下优点及有益效果：
本发明提供的阻燃母粒应用于制备木塑复合材料，能够获得较好的阻燃效果，产品防火性能好，燃烧过程黑烟和有毒害气体释放量小，提升了安全性能，应用前景好。
附图说明
图1为本发明阻燃母粒的制备路线图。
具体实施方式
以下结合具体实施例和附图来进一步说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明，本发明所用试剂和材料均为市购。
实施例1：
如图1所示，新型阻燃母粒的制备如下：
1、针状改性氢氧化镁的制备
将一定质量的水氯镁石经过溶解配制成1.5mol/L的氯化镁溶液，并取30ml上述溶液缓慢滴加到含有表面活性剂/分散剂的120ml 0.8mol/L的NaOH溶液的三口烧瓶中，表面活性剂/分散剂为硬脂酸钠/聚乙二醇1000，且添加量为氢氧化镁理论产量的3％，整个反应在高速条件下进行，直至氯化镁滴加完全。反应结束后在高速搅拌状态下将混合液陈化2h，85℃水浴加热搅拌6h然后进行过滤洗涤直至产物中不含有氯离子，并将产物置于115℃左右干燥4小时，得到针状形貌的改性氢氧化镁。
2、改性炭黑的制备
将钛酸酯偶联剂101(DN-101)5g加入到100ml的无水乙醇中，充分搅拌均匀，得偶联剂水解液；再将10g的未经改性的炭黑(充分干燥)与偶联剂水解液倒入三口烧瓶中，超声分散20min，80℃水浴加热搅拌6h，反应物经离心分离，用乙醇洗涤数次后，将所得炭黑置于110℃烘箱中干燥6h得改性炭黑，并密封保存。
3、改性聚磷酸铵(M-APP)的制备
将2ml的KH550偶联剂加入到150ml的无水乙醇中，充分搅拌均匀得偶联剂水解液，再将100g的未经改性的聚磷酸铵(充分干燥)与偶联剂水解液倒入三口烧瓶中超声分散15min，80℃水浴加热搅拌6h，反应物经离心分离，用乙醇洗涤数次后，将所得聚磷酸铵置于110℃烘箱中干燥4h得改性聚磷酸铵。
4、新型阻燃母粒的制备
将PVC树脂、八钼酸铵、针状改性氢氧化镁、改性炭黑、M-APP按照一定质量比先预混干燥完全，再通过双螺杆挤出机造粒得到新型阻燃母粒。
实施例1步骤4中组分的质量比为PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP＝55:0:15:15:15；
5、两步挤出法制备木塑产品，主要包括两个工艺流程：混炼造粒工艺以及挤出成型工艺。混炼造粒工艺：首先将木粉以及钙粉经过前处理，并与PVC树脂、除发泡剂之外的预混好的其它助剂在高速混炼机内混合2h，冷却至一定温度，再将发泡剂加入其中进行冷混，直至混合均匀进行双螺杆挤出机造粒，得到木塑母粒。
共挤成型工艺：将新型阻燃母粒、木塑母粒经过恒温干燥箱充分干燥，并通过带有特定模具的单螺杆挤出机进行共挤，定型，通过冷却水进行冷却，切割，得到pvc木塑制品。
实施例1～6中各组分含量及配比见表1所示：(表1中各组分均以份数计)
实施例2：方法同实施例1，不同的是实施例1步骤4中PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP质量比＝55:10:10:10:15。
实施例3：方法同实施例1，不同的是实施例1步骤4中PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP质量比＝55:15:10:10:10。
实施例4：方法同实施例1，不同的是实施例1步骤4中PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP质量比＝55:10:15:10:10。
实施例5：方法同实施例1，不同的是实施例1步骤4中PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP质量比＝55:10:20:10:5。
实施例6：方法同实施例1，不同的是实施例1步骤4中PVC：八钼酸铵：针状改性氢氧化镁：改性炭黑：M-APP质量比＝55:5:10:15:15。
性能测试：
冲击性能测试标准：GB/T 1043-1993；拉伸性能测试标准：GB/T 1040-1992；
平均烟气温度测试标准：GB/T 8625-2005；烟密度等级测试标准：GB/T 8627-1999；
极限氧指数测试标准：GB/T 2406.2-2009；燃烧性能等级测试：GB/T 8624-2012；
实施例1～6中制备得到的木塑材料性能见表2所示：
表2
对比例1：方法同实施例1，不同的是实施例1中采用的是未改性的氢氧化镁、炭黑和聚磷酸铵。
对比例2：方法同实施例1，不同的是实施例1中采用的是未改性的氢氧化镁和炭黑。
对比例3：方法同实施例1，不同的是实施例1中采用的是未改性的氢氧化镁和聚磷酸铵。
对比例4：方法同实施例1，不同的是实施例1中采用的是未改性的炭黑。
对比例1～4采用实施例1中的性能测试方法，结果见表3所示：
表3
采用市售常见的几种木塑材料，测定性能，具体见表4所示：
表4

Claims (10)

1.一种阻燃母粒，其特征在于，包括如下按重量份数计的组分制成：
PVC树脂 40~70
八钼酸铵 0~30
改性氢氧化镁 5~30
改性炭黑 5~30
改性聚磷酸铵 5~30；
所述改性氢氧化镁采用表面活性剂和分散剂与氯化镁反应后获得；
所述改性炭黑采用偶联剂A和炭黑反应获得；
所述改性聚磷酸铵采用偶联剂B与聚磷酸铵反应后所得。
2.根据权利要求1所述的阻燃母粒，其特征在于，所述偶联剂A为γ-（甲基丙烯酰氧）丙基三甲氧基硅烷、N,N'=双(2-甲基-2-硝基两基)-1.6-二氨基己烷、异丙基二油酸酰氧基钛酸酯或双-[γ-(三乙氧基硅)丙基] 四硫化物，所述偶联剂B为有机硅偶联剂、γ-（甲基丙烯酰氧）丙基三甲氧基硅烷、γ―氨丙基三乙氧基硅烷或焦磷酸型单烷氧基钛酸酯。
3.根据权利要求1所述的阻燃母粒，其特征在于，将氯化镁溶液滴加到含有表面活性剂和分散剂的NaOH溶液中，滴加完后陈化一定时间，水浴加热，过滤洗涤，干燥即得改性氢氧化镁，表面活性剂和分散剂的添加总量占改性氢氧化镁生成量的2.5~3.5%。
4.根据权利要求3所述的阻燃母粒，其特征在于，所述表面活性剂为硬脂酸钠或十二烷基苯磺酸钠，所述分散剂为聚乙二醇1000。
5.根据权利要求1所述的阻燃母粒，其特征在于，将偶联剂A加入到乙醇中，加入炭黑，超声，水浴加热，离心，洗涤，干燥后即得所述改性炭黑，偶联剂A与炭黑的混合质量比为1：（1~3）。
6.根据权利要求5所述的阻燃母粒，其特征在于，偶联剂A为钛酸酯偶联剂101。
7.根据权利要求1所述的阻燃母粒，其特征在于，将偶联剂B加入到乙醇中，加入聚磷酸铵，超声，水浴加热，离心，洗涤，干燥后即得所述改性聚磷酸铵，偶联剂B与聚磷酸铵的混合固液比为1：（40~60）。
8.根据权利要求1所述的阻燃母粒，其特征在于，偶联剂B为KH550。
9.一种阻燃型PVC木塑墙板，其特征在于，包括权利要求1至8任一所述的阻燃母粒。
10.根据权利要求9所述的阻燃型PVC木塑墙板，其特征在于，包括如下按重量份数计的组分制成：
PVC 45-55
木粉 5~25
钙粉 5~15
阻燃母粒 0.5~2
发泡剂 0.2~0.7
发泡调节剂 1~5
润滑剂 0.5~5
稳定剂 1~5
色粉 0.5~2.5。
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