CN114573877A - 一种吸附降解有机挥发物的组合物及母粒 - Google Patents
一种吸附降解有机挥发物的组合物及母粒 Download PDFInfo
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- CN114573877A CN114573877A CN202210246527.7A CN202210246527A CN114573877A CN 114573877 A CN114573877 A CN 114573877A CN 202210246527 A CN202210246527 A CN 202210246527A CN 114573877 A CN114573877 A CN 114573877A
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- Prior art keywords
- tetracarboxyl
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- porous material
- parts
- polyvinyl alcohol
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了一种吸附降解有机挥发物的组合物及母粒,该组合物以质量计包括多孔材料负载四羧基金属酞菁形成的复合颗粒10‑20份、改性聚乙烯醇5‑15份,本方案中利用多孔材料吸附有机挥发物,以含磺酸基团的改性聚乙烯醇吸水,多孔材料负载的四羧基金属酞菁在氧气、水分条件下将有机挥发物催化氧化降解成二氧化碳、水及小分子等无害物质,可重复循环进行,在上述物料比例下,吸附降解效果好,对于本吸附降解有机挥发物的组合物的应用,如直接与树脂等材料等混合形成母粒,可根据需求应用至家居、车载等领域。
Description
技术领域
本发明涉及材料技术领域,具体涉及一种吸附降解有机挥发物的组合物,以及包括上述吸附降解有机挥发物的组合物的汽车内饰用除味母粒。
背景技术
目前,高分子材料在家居、车载及厂房等多领域得到广泛应用,而大部分高分子材料受合成工艺等影响,都会不同程度地释放出有害的挥发性有机物(VOC),影响室内或车内空气质量,威胁人体健康,使高分子材料的应用受到限制。
以汽车用内饰材料为例,汽车内饰大部分采用高分子材料,如PP、PC、ABS、PVC等材料。其释放出有害的挥发性有机物(VOC),影响车内空气质量,威胁人体健康。2011年,环保部和国家质检总局联合制定的强制性国标GB/T 27630—2011《乘用车内空气质量评价指南》中规定了车内空气中苯、甲苯、二甲苯、乙苯、苯乙烯、甲醛、丙烯醛的浓度要求,强化了车内空气质量的管控。
目前对于减少高分子材料中的挥发物组分的典型方法包括:物理吸附法,如在高分子材料中添加沸石、活性炭、分子筛、硅藻土等,在高分子材料加工过程中添加可以物理吸附的无机材料进行吸附,添加量大,影响高分子材料的加工和应用性能。另一种是在高分子材料加工过程中添加汽提剂以通过真空抽提的方法减少挥发物,对减少的有机物挥发量有限,效果不佳。
中国专利申请号201811615208.9公布了一种除味母粒及其制备方法和应用,该方法将树脂、金属有机化合物、增容剂及助剂混合后,采用双螺杆挤出机共混造粒制备除味母粒,该方法采用的有机金属化合物为乙酰丙酮氧钒配合物、卤代卟啉铁配合物、二元羧酸(多元羧酸)与锌(或铜)的配合物的一种或多种的混合物,利用有机金属化合物在固相条件下实现活化有机挥发性化合物的作用,又可以吸附有机挥发性化合物,从而降低高分子材料的气味和TVOC的含量。虽然该母粒可以固相活化有机挥发性化合物,但没有明确有机挥发物降解成二氧化碳、水及小分子等无害物质。
中国专利申请号201611160803.9公布了一种低气味低雾化可用于汽车内饰的TPE材料及其制备方法,该方法在配方中加入汽提剂,使体系内有气味的低分子量物质与汽提剂中的低沸点溶剂相似相容,起到萃取TPE中气味性低分子量物质的作用,从而降低了VOCs含量及气味。
中国专利申请号201510130885.1公开了一种除味母粒及其制备方法和应用,该方法制备的母粒中含多孔性聚合物珠粒和汽提剂,汽提剂以游离态存在于多孔性聚合物珠粒的空隙中,两者之间通过共价键或范德华力相似相容原理加以结合。将该除味母粒添加到同种基体材料中,经螺杆挤出机的剪切分散,母粒中的汽提剂与聚合物中的VOC充分混合溶解,经螺杆下端抽真空处理,汽提剂与VOC一起被抽提到机筒外部,从而得到低气味的聚合物颗粒。
采用汽提剂作为降低聚合物颗粒中的低分子量有机挥发物,除气味的效果有限,制备的低气味的聚合物颗粒存在汽提剂没有去除干净,则重新引入其它的有机挥发物,另一方面,汽提剂的作用为一次性,在制备材料过程中提取一部分有机挥发物,残留的有机挥发物在制备成内饰后依旧存在。
发明内容
为解决上述至少一个技术缺陷,本发明提供了如下技术方案:
本申请文件公开一种吸附降解有机挥发物的组合物,以质量计,包括多孔材料负载四羧基金属酞菁形成的复合颗粒10-20份、改性聚乙烯醇5-15份,以2-丙烯酰胺-2-甲基丙磺酸或对苯乙烯磺酸钠与N,N'-乙烯基双丙烯酰胺、聚乙烯醇在质量比例3-6:0.5-2:10下共聚形成改性聚乙烯醇,多孔材料与四羧基金属酞菁的质量比为100:0.5-2。
本方案中利用多孔材料吸附有机挥发物,以含磺酸基团的改性聚乙烯醇吸水,多孔材料负载的四羧基金属酞菁在氧气、水分条件下将有机挥发物催化氧化降解成二氧化碳、水及小分子等无害物质,可重复循环进行,在上述物料比例下,吸附降解效果好。
其中N,N'-乙烯基双丙烯酰胺既是一种共聚单体,也是一种交联剂。若共聚改性聚乙烯醇没有交联,则吸水率太大;若交联度太大,则吸水率偏低,影响催化氧化效率。
对于本吸附降解有机挥发物的组合物的应用,如直接与树脂、或其他材料等混合注塑成型,可根据需求应用至家居、车载等领域。
进一步,所述多孔材料为二氧化硅、二氧化钛、沸石、硅藻土、玻璃微珠、分子筛的一种或多种,经试验,上述多孔材料吸附效果好,且较为常用,来源广泛,可单一选用二氧化硅、二氧化钛等,也可复合使用,如二氧化硅与二氧化钛1:1搭配,二氧化硅与沸石1:2搭配,沸石与硅藻土2:1搭配,硅藻土与玻璃微珠、分子筛按照1:1:1复合搭配等均可,在本司的实验下,吸附除味效果基本一致。
进一步,所述多孔材料的粒径50-70μm,孔径为1-5μm,应用时,如粒径50μm配合孔径1-2μm,粒径70μm搭配孔径4-5μm,粒径60μm搭配孔径3μm,粒径40μm搭配孔径2±0.5μm等,上述粒径范围、孔径范围为本司试验后得到的优选范围,可更好地负载四羧基金属酞菁以及吸附有机挥发物。
进一步,所述四羧基金属酞菁为四羧基铁酞菁、四羧基钴酞菁、四羧基锌酞菁、四羧基铜酞菁的一种或多种,同样可以四羧基铁酞菁、四羧基钴酞菁复合搭配,如质量比1:1,1:2,1:3等,或四羧基锌酞菁、四羧基铜酞菁复合搭配,如质量比1:1,1:3,2:1等,当然也可根据个人需求自由搭配,在本司的实验下,除味效果基本一致。
进一步,所述多孔材料负载四羧基金属酞菁形成的复合颗粒的制备:将多孔材料浸入四羧基金属酞菁的溶液中静置,之后将多孔材料取出并浸入水中静置,自水中取出多孔材料并烘干后即得复合颗粒,多孔材料静置过程中,孔中的气泡被赶出,四羧基金属酞菁溶液进入,取出浸入水中使溶剂混溶于水,有助四羧基金属酞菁分子沉淀在多孔材料中,可用水多次浸泡或冲洗,烘干后即为复合颗粒。根据四羧基金属酞菁的性质,多以有机溶剂形成溶液,有机溶剂如二甲基乙酰胺(DMAC)、丙酮、DMF、甲苯、乙酸乙酯、氯仿等,优选采用DMAC。对于四羧基金属酞菁溶液的浓度,如1mg/ml,0.5mg/ml,1.5mg/ml等均可,浓度可调整,根据在不同溶剂中溶解度的不同自由选择,浓度高的四羧基金属酞菁溶液以多孔材料浸泡一次即可,浓度低的可选择浸泡多次,浸泡时间一般如3-5min,或10-20min,当然也可以更长时间浸泡。
进一步,2-丙烯酰胺-2-甲基丙磺酸或对苯乙烯磺酸钠与N,N'-乙烯基双丙烯酰胺、聚乙烯醇在引发剂作用下,在70-75℃下反应4-6h,提纯除杂后得到改性聚乙烯醇。对于改性聚乙烯醇的共聚采用引发剂引发聚合,引发剂如常用的过硫酸钾、亚硫酸氢钠等,对于提纯的方法如无无水乙醇多次洗涤即可,目的在于除去未反应的单体。
进一步,所述聚乙烯醇的分子量为10-20万。
本发明公开一种汽车内饰用除味母粒,包括上述的吸附降解有机挥发物的组合物以及树脂65-85份、抗氧化剂0.5-2份和润滑剂0.5-1份,以质量计。
本方案中将上述吸附降解有机挥发物的组合物应用至汽车内饰材料中,搭配上述比例的组分以更好地形成母粒,方便母粒与内饰材料的其他组分混合以及吸附消味,如可将母粒以质量比0.5-3%的质量比与树脂等内饰材料组分混合注塑成型所需的内饰,经试验可显著降低汽车内饰材料的气味和VOC含量。
进一步,所述树脂为PP、PE、PC、ABS、POE、OBC中的一种或多种。
进一步,所述母粒的制备过程如下:将吸附降解有机挥发物的组合物以及树脂65-85份、抗氧化剂0.5-2份和润滑剂0.5-1份进行混合,经熔融造粒制得母粒。如以螺杆挤出机挤出造粒,常见的造粒的方式。
与现有技术相比,本发明的有益效果:
1、本发明将含磺酸基团的改性聚乙烯醇与负载四羧基金属酞菁的多孔材料复合颗粒相配合以催化降解有机挥发物,重复循环吸附降解,效果显著,可选择与树脂等混合应用至家具、车载等产品中以起到吸附降解的效果。
2、本发明将吸附组合物应用至车用内饰材料中,优选合适比例组分相搭配以更好地与内饰材料混合及吸附消味,经试验可显著降低内饰材料的气味和VOC含量。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
以下实施例中改性聚乙烯醇、复合颗粒的制备如下:
改性聚乙烯醇的制备
在250ml三口烧瓶中加入100ml水,加入10g聚乙烯醇,加热到90℃进行搅拌溶解,降温至室温,再加入3-6g的2-丙烯酰胺-2-甲基丙磺酸(或对苯乙烯磺酸钠)和0.5-2g的N,N'-乙烯基双丙烯酰胺及少量引发剂过硫酸钾和亚硫酸氢钠(过硫酸钾与亚硫酸氢钠之间的量比采用1:1,引发剂的加入量与聚乙烯醇等的比例为1:100),溶解并搅拌均匀,通氮气除氧30min,然后升温至72±0.5℃进行共聚,反应全程氮气保护,反应5h后体系呈凝胶状,取出干燥至恒重,粉碎,再用无水乙醇洗涤、干燥得到白色固体颗粒,粉碎并用200目标准筛过滤,即得改性聚乙烯醇。同一物料组成比例在本方案反应温度、反应时间范围内制备的聚乙烯醇性能基本一致。
多孔材料负载四羧基金属酞菁的复合颗粒的制备
将四羧基金属酞菁溶于DMAC中,配置成1mg/ml的DMAC溶液,将多孔材料(粒径50-70μm,孔径1-5μm)浸入到DMAC溶液中,时间0.5-2h,多孔材料内部的气泡被充分赶出后,溶液充满多孔材料的孔体积,将样品取出后浸泡在清水中,时间0.5h,多次洗涤样品后烘干即得多孔材料负载四羧基金属酞菁的复合颗粒,四羧基金属酞菁负载量(wt%)为0.5-2%。上述孔径、粒径范围的多孔材料对产品的吸附影响基本一致。
实施例1
将POE 75份、多孔二氧化硅负载四羧基铜酞菁的复合颗粒15份(负载量为0.8wt%)、改性聚乙烯醇10份、抗氧化剂1份和润滑剂1份进行混合,再经双螺杆挤出机进行熔融共混造粒,即得汽车内饰用除味母粒。
将汽车内饰用除味母粒按照2%的质量比添加到POE材料中,采用双螺杆挤出机进行熔融共混挤出造粒,注塑成型低气味POE材料产品,造粒及注塑参数设置依据常规即可。
其中改性聚乙烯醇(型号:PVA235,分子量为18-20万)在制备过程中,2-丙烯酰胺-2-甲基丙磺酸、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为5:1.2:10。
实施例2:
母粒组成:ABS 80份、多孔二氧化钛负载四羧基铁酞菁的复合颗粒10份(负载量为1.5wt%)、改性聚乙烯醇15份、抗氧化剂1份和润滑剂1份。
将汽车内饰用除味母粒按照1%的质量比添加到ABS材料中,注塑成型低气味ABS材料产品。
其中改性聚乙烯醇(型号:PVA2899L,分子量为12-13万)在制备过程中,对苯乙烯磺酸钠、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为6:2:10。
实施例3:
母粒组成:PC 75份、多孔沸石珠负载四羧基钴酞菁的复合颗粒10份(负载量为2wt%)、改性聚乙烯醇8份、抗氧化剂1份和润滑剂1份。
将汽车内饰用除味母粒按照1.5%的质量比添加到PC材料中,注塑成型低气味PC材料产品。
其中改性聚乙烯醇(型号:PVA3099L,分子量为13-15万)在制备过程中,对苯乙烯磺酸钠、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为3:1:10。
实施例4:
母粒组成:PE 75份、多孔玻璃微珠负载四羧基钴酞菁的复合颗粒8份(负载量为0.5wt%)、多孔玻璃微珠负载四羧基铁酞菁的复合颗粒8份(负载量为0.5wt%),改性聚乙烯醇10份、抗氧化剂1.5份和润滑剂0.8份。
将汽车内饰用除味母粒按照2%的质量比添加到PE材料中,注塑成型低气味PE材料产品。
其中改性聚乙烯醇(型号:PVA3099L,分子量为13-15万)在制备过程中,对苯乙烯磺酸钠、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为3:1.5:10。
实施例5:
母粒组成:OBC 85份、多孔二氧化硅负载四羧基铁酞菁的复合颗粒5份(负载量为1wt%),多孔二氧化钛负载四羧基锌酞菁的复合颗粒5份(负载量为1.5wt%)、改性聚乙烯醇15份、抗氧化剂1份和润滑剂1份。
将汽车内饰用除味母粒按照2%的质量比添加到POE材料中,注塑成型低气味POE材料产品。
其中改性聚乙烯醇(型号:PVA2899L,分子量为12-13万)在制备过程中,对苯乙烯磺酸钠、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为4:0.8:10。
实施例6:
母粒组成:PP 65份、多孔玻璃微珠负载四羧基钴酞菁的复合颗粒4份(负载量为0.5wt%)、多孔玻璃微珠负载四羧基铁酞菁的复合颗粒3份(负载量为0.5wt%),多孔玻璃微珠负载四羧基锌酞菁的复合颗粒3份(负载量为0.5wt%)、改性聚乙烯醇8份、抗氧化剂2份和润滑剂1份。
将汽车内饰用除味母粒按照2%的质量比添加到PP材料中,注塑成型低气味PP材料产品。
其中改性聚乙烯醇(型号:PVA235,分子量为18-20万)在制备过程中,2-丙烯酰胺-2-甲基丙磺酸、N,N'-乙烯基双丙烯酰胺和聚乙烯醇,重量比例为4:0.8:10。
对比例1:
将PP 65份、多孔玻璃微珠(同实施例6)10份,抗氧化剂2份和润滑剂1份进行混合,再经双螺杆挤出机进行熔融共混造粒,即得汽车内饰用除味母粒。将汽车内饰用除味母粒按照2%的质量比添加到PP材料中,采用双螺杆挤出机进行熔融共混挤出造粒得到低气味PP材料产品。
对比例2:
将PP 65份(重量份)、多孔玻璃微珠(同实施例6)25份,抗氧化剂2份和润滑剂1份进行混合,再经双螺杆挤出机进行熔融共混造粒,即得汽车内饰用除味母粒。将汽车内饰用除味母粒按照2%的质量比添加到PP材料中,采用双螺杆挤出机进行熔融共混挤出造粒得到低气味PP材料产品。
对上述实施例及对比例制备的产品进行性能的检测
性能测试方法:
1)TVOC测试:按照大众PV3341标准测试,测试样品为结构件的规定位置上截取重量为10-25mg小块,此过程中不能使样品受热,试样重量依据瓶的体积,10ml瓶容积1g±0.001g。测试结果见表1。
2)气味测试:按照大众PV3341标准测试,密闭容器中的试样于80℃下烘2h,后冷却到60℃。由5人以上参与评价,统计总的判断。1分为无气味,2分为有气味但无干扰性异味,3分为有明显气味但无干扰性异味,4分为干扰性异味,5分为有强烈干扰性异味,6分为有难以忍受的气味。测试结果见表1。
表1材料除味效果评价结果
从表1可以看出,本发明制备的除味母粒在实际使用中添加量少就可以得到很好的降低气味和TVOC指标效果,远优于对比例1和对比例2。添加本发明制备的除味母粒后,能够满足汽车内饰对气味的严格要求。
以上仅是本发明的优选实施方式,本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种吸附降解有机挥发物的组合物,其特征在于,以质量计,包括多孔材料负载四羧基金属酞菁形成的复合颗粒10-20份、改性聚乙烯醇5-15份,以2-丙烯酰胺-2-甲基丙磺酸或对苯乙烯磺酸钠与N,N'-乙烯基双丙烯酰胺、聚乙烯醇在质量比例3-6:0.5-2:10下共聚形成改性聚乙烯醇,多孔材料与四羧基金属酞菁的质量比为100:0.5-2。
2.如权利要求1所述的一种吸附降解有机挥发物的组合物,其特征在于:所述多孔材料为二氧化硅、二氧化钛、沸石、硅藻土、玻璃微珠、分子筛的一种或多种。
3.如权利要求2所述的一种吸附降解有机挥发物的组合物,其特征在于:所述多孔材料的粒径50-70μm,孔径为1-5μm。
4.如权利要求1所述的一种吸附降解有机挥发物的组合物,其特征在于:所述四羧基金属酞菁为四羧基铁酞菁、四羧基钴酞菁、四羧基锌酞菁、四羧基铜酞菁的一种或多种。
5.如权利要求1所述的一种吸附降解有机挥发物的组合物,其特征在于:所述多孔材料负载四羧基金属酞菁形成的复合颗粒的制备:将多孔材料浸入四羧基金属酞菁的溶液中静置,之后将多孔材料取出并浸入水中静置,自水中取出多孔材料并烘干后即得复合颗粒。
6.如权利要求1所述的一种吸附降解有机挥发物的组合物,其特征在于:2-丙烯酰胺-2-甲基丙磺酸或对苯乙烯磺酸钠与N,N'-乙烯基双丙烯酰胺、聚乙烯醇在引发剂作用下,在70-75℃下反应4-6h,提纯除杂后得到改性聚乙烯醇。
7.如权利要求1所述的一种吸附降解有机挥发物的组合物,其特征在于:所述聚乙烯醇的分子量为10-20万。
8.一种汽车内饰用除味母粒,其特征在于,包括上述权利要求1-7中任一项所述的吸附降解有机挥发物的组合物以及树脂65-85份、抗氧化剂0.5-2份和润滑剂0.5-1份,以质量计。
9.如权利要求8所述的一种汽车内饰用除味母粒,其特征在于:所述树脂为PP、PE、PC、ABS、POE、OBC中的一种或多种。
10.如权利要求8所述的一种汽车内饰用除味母粒,其特征在于:所述母粒的制备过程如下:将吸附降解有机挥发物的组合物以及树脂65-85份、抗氧化剂0.5-2份和润滑剂0.5-1份进行混合,经熔融造粒制得母粒。
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