CN111848989A - 一种含有机添加剂微塑料及其制备方法 - Google Patents
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Abstract
一种含有机添加剂微塑料及其制备方法，包括以下步骤：（1）将特定的溶剂溶解购得的商品化微塑料；（2）向溶解液中加入增塑剂、阻燃剂等有机物添加剂并混合均匀；（3）将溶解液加入到容器中，待溶剂挥发后可得到含有机添加剂塑料薄片，也可在搅拌下将水加入到溶解液中，使塑料沉淀析出，可制得含有机添加剂的微塑料；（4）将上述得到的塑料薄片剪碎后，加入液氮，用粉碎机粉碎或研钵磨碎，过不同粒径的金属网筛，可制得不同粒径的含有机添加剂的片状微塑料，将步骤（3）得到的微塑料加入液氮，研磨过筛后可得更小粒径含有机添加剂的微塑料。通过本方法可以方便的制备含不同有机添加剂的微塑料，为系统研究含添加剂微塑料的环境行为和生态风险提供基础材料。
Description
技术领域
本发明属于环境科学领域，具体涉及一种含有机添加剂微塑料的制备方法，可用于研究环境中含有机添加剂微塑料的环境行为和生态风险。
背景技术
微塑料是指尺寸小于5 毫米的塑料微粒，主要来源于大块塑料的破碎和日化用品中磨砂颗粒的排放。微塑料具有易迁移、易吸附和释放污染物、易被生物吞食等特性，对生态系统和人体健康具有严重的潜在危害。为了满足加工和应用需求，塑料在加工过程中通常需要加入不同种类的化学助剂如增塑剂、阻燃剂、稳定剂、抗菌剂、着色剂和填充剂等。比如聚烯烃类塑料因阻燃性低而常需加入阻燃剂，聚氯乙烯塑料因质地脆硬而常需加入增塑剂。在过去几年里，添加剂在微塑料土壤生物效应中的作用和贡献并未受到充分关注，但基于其他环境体系的研究显示，添加剂释放可能在微塑料导致的生物毒性效应中发挥着至关重要的作用。
目前试剂公司提供的微塑料多为不含添加剂的微塑料，市场流通的塑料成分复杂且不明确，很难通过常规粉碎塑料的方法制备含特定添加剂种类和浓度的微塑料。工厂生产含有机添加剂的塑料通常是通过常规的密炼工艺，将有机添加剂和塑料颗粒混合后成型挤出。但生产工艺较为复杂且不易将有机添加剂和塑料混合均匀，对于部分塑料如聚氯乙烯较难成型，且在高温下容易分解，需要加入大量热稳定剂等添加剂。近年来，也有部分专利报道了含某些荧光或发光材料微塑料的制备方法，如张宴等发明了一种制备颗粒状和薄片状荧光标记微塑料，主要通过密炼工艺制备（CN107160585A）；李战军等利用塑料的溶胀作用制备了一种长余辉发光纳米粒子标记的微塑料（CN108485097A）；李战军等还通过类似方法制备了一种金属有机荧光配合物标记的微塑料。但关于制备含塑化剂、阻燃剂等日常使用塑料中常见有机添加剂的微塑料的研究还未见报道。
发明内容
解决的技术问题：本发明一种含有机添加剂微塑料及其制备方法，解决了难以通过直接购买或简单粉碎获得含有特定种类和浓度的微塑料，可用于研究含添加剂微塑料的环境行为和生态风险。
技术方案：一种含有机添加剂微塑料的制备方法，包括如下步骤：（1）称取粒径<5毫米的商品化微塑料颗粒，将微塑料颗粒缓慢加入到装有有机溶剂的容器中并搅拌，得到澄清的塑料溶解液；所述微塑料颗粒与有机溶剂的质量比为1:（5-20）；（2）称取有机添加剂，将有机添加剂加入到塑料溶解液中，并搅拌均匀，所述有机添加剂为固体时，加入有机溶剂使其溶解；所述有机添加剂为液体时，直接添加；（3）吸取步骤（2）所得的塑料溶解液到容器中展开成均匀厚度的液体，放入通风橱中，待溶剂挥发后制得塑料薄膜；或将水倒入步骤（2）制得塑料溶解液中，使塑料沉淀析出，过滤，风干，制得含添加剂的微塑料；（4）将步骤（3）制得塑料薄膜用水清洗后自然晾干，将塑料薄膜剪成条状塑料或剪碎后加入液氮，用粉碎机粉碎或研钵磨碎，过不同粒径的金属网筛，制得不同粒径的含有机添加剂片状微塑料颗粒；或将步骤（3）所得含添加剂的微塑料颗粒加入液氮粉碎，制得更小粒径含有机添加剂微塑料颗粒。
上述微塑料的材质包括但不仅限于聚氯乙烯、聚乙烯、聚丙烯或聚苯乙烯；有机溶剂包括但不仅限于四氢呋喃、二甲基亚砜、环己酮、丙酮、乙酸乙酯、乙醚中的至少一种，可溶解相应材质的塑料。
上述步骤（1）中微塑料颗粒与有机溶剂的质量比为1:（5-20）。
上述步骤（2）中的有机添加剂包括但不仅限于邻苯二甲酸酯、多溴联苯醚、双酚A中的至少一种，添加剂含量为0.1-70%。
上述步骤（3）中塑料薄膜厚度<5毫米，塑料颗粒直径<5毫米。
上述步骤（4）中条状微塑料的长度和宽度<5毫米，用粉碎机粉碎的时间>1分钟，<10分钟，研钵研磨时间>20分钟，金属筛目数大于4目。
上述制备方法制得的含有机添加剂微塑料。
有益效果：本发明过程简单，有机添加剂种类、数量、浓度易于控制，有机添加剂与塑料基体混合均匀，制备过程不易混入其他杂质，操作简单，在实验室及工厂都易于小规模生产，生产成本低，可制备出含有所需有机添加剂的不同粒径的微塑料颗粒，为含添加剂微塑料的实验室研究提供了洁净的材料样品。
附图说明
图1为实施例1中所制得含有机添加剂微塑料薄膜；
图2为实施例1中将薄膜剪成1厘米ⅹ1厘米左右尺寸；
图3为实施例1中所得含有机添加剂片状微塑料；
图4为实施例1中所得含有机添加剂片状微塑料红外显微图片（长度约为0.5 mm）；
图5为实施例1中含邻苯二甲酸二(2-乙基）己酯（DEHP）增塑剂聚氯乙烯（PVC）微塑料红外图谱，加入DEHP添加剂后，PVC微塑料的红外谱图中出现DEHP的红外峰，说明DEHP成功添加到PVC微塑料中；
图6为实施例3中含1% 2,2',4,4'-四溴联苯醚聚丙烯片状微塑料用正己烷提取后，气相色谱（电子捕获检测器）检测后的图谱，经与标准样品对照后确认为2,2',4,4'-四溴联苯醚，说明2,2',4,4'-四溴联苯醚成功添加到聚丙烯微塑料中；
图7为实施例4中将水倒入塑料溶解液中形成的微塑料悬浊液。
具体实施方式
实施例1：含5%邻苯二甲酸二(2-乙基）己酯增塑剂的片状聚氯乙烯微塑料制备
（1）向烧杯中加入100毫升四氢呋喃，在玻璃棒搅拌下加入9.5克商品化聚氯乙烯（粒径<2毫米），得到澄清的聚氯乙烯溶液。
（2）称取0.5 克邻苯二甲酸二(2-乙基）己酯，加入到上述的聚氯乙烯溶液中，搅拌均匀。
（3）用移液枪吸取10毫升溶液到直径为9 厘米的玻璃皿中，震荡使溶液高度均匀，放入通风橱中一小时，待有机溶液挥发后得到邻苯二甲酸二(2-乙基）己酯添加浓度为5%，厚度约为0.3毫米的聚氯乙烯塑料膜。
（4）将步骤（3）所得薄膜剪成1厘米ⅹ1厘米左右条状尺寸，放入粉碎机中，加入液氮至浸没。每次粉碎30秒，粉碎10次，得到含5%邻苯二甲酸二(2-乙基）己酯聚氯乙烯微塑料。
（5）将步骤（4）所得微塑料过10目金属筛，得到微塑料尺寸<1.7毫米的含5%邻苯二甲酸二(2-乙基）己酯片状聚氯乙烯微塑料。
实施例2：含20%邻苯二甲酸二辛酯增塑剂的片状聚氯乙烯微塑料制备
（1）向烧杯中加入160毫升四氢呋喃，在玻璃棒搅拌下加入8克商品化聚氯乙烯（粒径<2毫米），得到澄清的聚氯乙烯溶液。
（2）称取2 克邻苯二甲酸二辛酯，加入到上述的聚氯乙烯溶液中，搅拌均匀。
（3）用移液枪吸取10 mL溶液到直径为9 厘米的玻璃皿中，震荡使溶液高度均匀，放入通风橱中一小时，待有机溶液挥发后得到邻苯二甲酸二辛酯添加浓度为20%，厚度约为0.15毫米的聚氯乙烯塑料膜。
（4）将步骤（3）所得薄膜剪成1厘米ⅹ1厘米左右条状尺寸，放入粉碎机中，加入液氮至浸没。每次粉碎30秒，粉碎10次，得到含20%邻苯二甲酸二辛酯聚氯乙烯微塑料。
（5）将步骤（4）所得微塑料过10目金属筛，得到微塑料尺寸<1.7毫米的含20%邻苯二甲酸二辛酯片状聚氯乙烯微塑料。
实施例3 含1% 2,2',4,4'-四溴联苯醚聚丙烯片状微塑料的制备
（1）向烧杯中加入87毫升二甲基亚砜，10毫升环己酮和3毫升乙酸乙酯，在玻璃棒搅拌下加入5克商品化聚丙烯（粒径<1毫米），得到澄清的聚丙烯溶液。
（2）称取0.05 克2,2',4,4'-四溴联苯醚加入到装有10毫升正己烷的玻璃瓶中，待2,2',4,4'-四溴联苯醚溶解后加入到上述的聚丙烯溶液中，搅拌均匀。
（3）用移液枪吸取5 mL溶液到直径为9 厘米的玻璃皿中，震荡使溶液高度均匀，放入通风橱中一小时，待有机溶液挥发后得到2,2',4,4'-四溴联苯醚添加浓度为1%，厚度为0.15毫米的聚丙烯塑料膜。
（4）将步骤（3）所得薄膜剪成1厘米ⅹ1厘米左右条状尺寸，放入研钵中，加入液氮至浸没。研磨30分钟，得到含1%2,2',4,4'-四溴联苯醚聚丙烯微塑料。
（5）将步骤（4）所得微塑料过20目金属筛，得到微塑料尺寸<0.83毫米的含1%2,2',4,4'-四溴联苯醚片状聚丙烯微塑料。
实施例4：含5%邻苯二甲酸二(2-乙基）己酯增塑剂的聚氯乙烯微塑料制备
（1）向烧杯中加入50毫升四氢呋喃，在玻璃棒搅拌下加入9.5克商品化聚氯乙烯（粒径<2毫米），得到澄清的聚氯乙烯溶液。
（2）称取0.5 克邻苯二甲酸二(2-乙基）己酯，加入到上述的聚氯乙烯溶液中，搅拌均匀。
（3）吸取20毫升水滴加到塑料溶解液中，滴加过程搅拌，将所得浑浊液过滤，风干，制得粒径<5毫米含5%邻苯二甲酸二(2-乙基）己酯聚氯乙烯微塑料。
（4）将步骤（3）所得微塑料放入粉碎机中，加入液氮至浸没。每次粉碎30秒，粉碎10次，得到含5%邻苯二甲酸二(2-乙基）己酯聚氯乙烯微塑料。
（5）将步骤（4）所得微塑料过20目金属筛，得到微塑料尺寸<0.83毫米的含5%邻苯二甲酸二(2-乙基）己酯聚氯乙烯微塑料。
本发明实施例中虽然只用到了邻苯二甲酸二(2-乙基）己酯、邻苯二甲酸二辛酯、2,2',4,4'-四溴联苯醚三种添加剂和聚氯乙烯、聚丙烯两种高分子材料，但是同领域技术人员很容易找到其它类型有机添加剂和高分子材料替代实施例中用到这几种材料，也是本发明保护范围之内。
Claims (7)
1.一种含有机添加剂微塑料的制备方法，其特征在于包括如下步骤：（1）称取粒径<5毫米的商品化微塑料颗粒，将微塑料颗粒缓慢加入到装有有机溶剂的容器中并搅拌，得到澄清的塑料溶解液；所述微塑料颗粒与有机溶剂的质量比为1:（5-20）；（2）称取有机添加剂，将有机添加剂加入到塑料溶解液中，并搅拌均匀，所述有机添加剂为固体时，加入有机溶剂使其溶解；所述有机添加剂为液体时，直接添加；（3）吸取步骤（2）所得的塑料溶解液到容器中展开成均匀厚度的液体，放入通风橱中，待溶剂挥发后制得塑料薄膜；或将水倒入步骤（2）制得塑料溶解液中，使塑料沉淀析出，过滤，风干，制得含添加剂的微塑料；（4）将步骤（3）制得塑料薄膜用水清洗后自然晾干，将塑料薄膜剪成条状塑料或剪碎后加入液氮，用粉碎机粉碎或研钵磨碎，过不同粒径的金属网筛，制得不同粒径的含有机添加剂片状微塑料颗粒；或将步骤（3）所得含添加剂的微塑料颗粒加入液氮粉碎，制得更小粒径含有机添加剂微塑料颗粒。
2.根据权利要求1所述含有机添加剂微塑料的制备方法，其特征在于所述微塑料的材质包括但不仅限于聚氯乙烯、聚乙烯、聚丙烯或聚苯乙烯；有机溶剂包括但不仅限于四氢呋喃、二甲基亚砜、环己酮、丙酮、乙酸乙酯、乙醚中的至少一种，可溶解相应材质的塑料。
3.根据权利要求1所述含有机添加剂微塑料的制备方法，其特征在于所述步骤（1）中微塑料颗粒与有机溶剂的质量比为1:（5-20）。
4.根据权利要求1所述含有机添加剂微塑料的制备方法，其特征在于所述步骤（2）中的有机添加剂包括但不仅限于邻苯二甲酸酯、多溴联苯醚、双酚A中的至少一种，添加剂含量为0.1-70%。
5.根据权利要求1所述含有机添加剂微塑料的制备方法，其特征在于所述步骤（3）中塑料薄膜厚度<5毫米，塑料颗粒直径<5毫米。
6.根据权利要求1所述含有机添加剂微塑料的制备方法，其特征在于所述步骤（4）中条状微塑料的长度和宽度<5毫米，用粉碎机粉碎的时间>1分钟，<10分钟，研钵研磨时间>20分钟，金属筛目数大于4目。
7.权利要求1-6任一所述制备方法制得的含有机添加剂微塑料。
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