CN112940030B - 一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法 - Google Patents
一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法 Download PDFInfo
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Abstract
本发明公开了一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法。该方法包括以下步骤：1）对废弃偏光膜进行破碎，过5~100目筛后置于封口袋中备用；2）取适量样品置于萃取容器中后放入微波萃取仪中，加入适量萃取溶剂，所述萃取溶剂体积为萃取容器体积的1/3‑2/3，微波功率200‑500 W，萃取温度为35~75℃，萃取时间为15‑50 min，制得提取液；3）将提取液进行抽滤，获得滤液，将滤液旋转蒸发除去溶剂，制得产品，即环保型无卤阻燃剂。本发明通过采用微波萃取可高效提取偏光膜中的无卤阻燃剂，且操作简单、耗时短，为环保型磷系阻燃剂回收研究打下基础。
Description
技术领域
本发明属于提取制备技术领域，更具体的说，涉及一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法。
背景技术
我国大量废弃液晶面板（LCD）产品将经过部分企业的分拣、分类、测试、重装、关键部件翻新（如偏光膜）等工艺进入再制造和降级利用阶段，在这一过程中存在大量偏光膜的废弃，偏光膜是一种具有偏光性能的塑料薄膜，主要成分是三醋酸纤维素（CTA）、磷酸三苯酯（TPP）和聚乙烯醇（PVA）。其中所含的TPP属于典型的磷系阻燃剂。磷系阻燃剂作为环保型无卤阻燃剂中重要的品种，具有稳定性好、挥发少、分解时低烟、低毒性等特点，具有阻燃和增塑双功能，在阻燃领域具有非常重要的地位。自20世纪70年代以来，有机磷酸酯阻燃剂在各种基于聚合物的工业和消费品中的使用量越来越大，例如电子产品、油漆、纺织品、家装材料、交通运输等行业，其用量仅次于卤系阻燃剂。
电子电器产品中阻燃剂的回收方法主要为萃取，包括索氏萃取、超声波萃取、超临界萃取、微波辅助萃取和快速溶剂萃取等，国家质检总局发布标准和电子行业标准均采用索式萃取法。经检索，上述相关技术研究局限于从单一废印刷电路板原料中萃取磷系阻燃剂，或为已受到使用限制的有机溴系阻燃剂的提取，目前应用较多的索氏萃取法耗时久、效率低、萃取剂用量大、能耗高，不适合大规模工业化生产。然而，尚未有研究采用微波萃取法从偏光膜中提取磷系阻燃剂。微波萃取技术作为一种新兴的环保技术，在废弃物资源化、污染物检测等领域得到了广泛的应用。微波萃取可对萃取物中的不同组分进行选择性加热，从而使目标物质从体系中分离出来，提高萃取效率，缩短萃取时间。
发明内容
针对现有技术存在的缺陷，本发现的目的是提供一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法，该方法具有提取时间短、产物收率高、提取溶剂可重复使用等优点。
本发明提供一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法，包括以下步骤：
1）将人工拆解废弃液晶面板得到废弃偏光膜进行破碎，过5~100目筛后置于封口袋中备用；
2）取适量样品置于四颈圆底烧瓶后放入微波萃取仪中，加入适量萃取溶剂，料液比1:100-2:50 g·mL-1，微波功率200-500W，萃取温度为35~75℃，萃取时间为15-60 min，制得提取液；其中：萃取溶剂为甲醇、乙醇、丙酮、乙腈、乙酸乙酯、甲苯中一种或多种混合物
3）将提取液进行抽滤，获得滤液，将滤液旋转蒸发除去溶剂，制得产品。
优选的，步骤2）中，萃取溶剂为丙酮，料液比1:100-2:50 g·mL-1，微波功率200-300W，萃取温度为45~55℃，萃取时间为15-30 min。
优选的，步骤2）中，萃取溶剂体积为萃取容器体积的1/3-2/3。
优选的，步骤3）中，旋转蒸发温度为35~50 ℃。
优选的，步骤3）中，旋转蒸发过程中蒸出的溶剂即为萃取溶剂，可以重复使用。
和现有技术相比，本发明的有益效果在于：
本发明所述的偏光膜中无卤阻燃剂的微波萃取方法，能够高效的提取偏光膜中的无卤阻燃剂，在短时提取20min~30min的条件下，提取效率一般达到90%以上，甚至高达96.23%，远远高于传统的索氏萃取法。同时，操作简单，萃取温度低，耗时短，降低了能耗，萃取溶剂可重复利用，明显减少了污染物排放对环境的影响。此外，本发明方法得到的工艺参数为微波提取废弃偏光膜中的无卤阻燃剂的工业化引用提供了一定的指导意义，进而也为废弃LCD中有机物的资源化提供参考意义。
附图说明
图1为实施例1溶剂种类对磷酸三苯酯萃取效果的影响。
图2为实施例2温度对磷酸三苯酯萃取效果的影响。
图3为实施例3时间对磷酸三苯酯萃取效果的影响。
图4为实施例4料液比对磷酸三苯酯萃取效果的影响。
图5为气相色谱法-质谱法联用对产品表征结果。
图6为红外光谱法对产品表征结果。
具体实施方式
下面结合附图和具体实施例，对本发明的技术方案作进一步的描述，但本发明不局限于这些实施例。
对典型液晶显示产品的废弃笔记本电脑、台式电脑进行人工拆解，得到废弃液晶面板组件，再获取其中的偏光膜，对废弃偏光膜进行破碎，过60目筛后置于封口袋中备用。
气相色谱法-质谱法联标准曲线制作：准确称取0.1g磷酸三苯酯，用乙酸乙酯(HPLC)定容至100mL，后逐级稀释成适用浓度的标准溶液，采用气相色谱法-质谱法联用测定并绘制标准曲线。其中，气相色谱-质谱仪为7890B型GC串联5977B型MS(美国Agilent公司)，色谱柱：DB-5HT气相色谱柱（15.00m×0.25mm×0.1µm）。色谱柱升温程序：初温50℃，保留2分钟，以30℃/min升至200℃，保留2分钟，再以8℃/min升至260℃；载气（氦气，纯度≥99.999%）流速为1mL/min；进样口温度250℃，脉冲不分流进样；自动进样，进样体积为1µm；质谱条件：电子轰击离子源（EI）电压为70eV，离子源温度240℃，四极杆温度150℃，GC-MS接口温度为280℃；采集方式：全扫描(SCAN)，质荷比扫描范围为50-500；溶剂延迟：7.0min。
采用GC-MS、红外光谱法对产品进行表征，经验证为目标产物，结果如图5、6。
实施例1
取1g样品置于四颈圆底烧瓶后放入微波萃取仪中，分别加入50mL丙酮、乙醇、甲醇、乙腈、甲苯和甲醇混合溶液，其他条件相同：微波功率250W，萃取温度分别为55℃、70℃、60℃、75℃、60℃（依据沸点设定，常压微波萃取条件下，萃取温度低于沸点），萃取时间为20min，制得提取液。将提取液进行抽滤，获得滤液，将滤液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出的萃取剂可重复利用。将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂。计算磷酸三苯酯提取率分别为95.89%、62.08%、66.4%、62.35%、70.51%(图1)。
实施例2
取1g样品置于四颈圆底烧瓶后放入微波萃取仪中，加入50mL丙酮，微波功率250W，萃取时间为20min，萃取温度分别为35℃、45℃和55℃，制得提取液。将提取液进行抽滤，获得滤液，将滤液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出丙酮可重复利用；将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂。计算磷酸三苯酯提取率分别为81.23%、88.69%、95.89%（图2）。
实施例3
取1g样品置于四颈圆底烧瓶后放入微波萃取仪中，加入50mL丙酮，微波功率250W，萃取温度为55℃，萃取时间分别为25min、30min，制得提取液。将提取液进行抽滤，获得滤液，将滤液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出丙酮可重复利用；将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂。计算磷酸三苯酯提取率为95.93%、96.23%（图3）。
实施例4
分别取0.5g、1.5g、2.0g样品置于四颈圆底烧瓶后放入微波萃取仪中，其他条件相同：50mL丙酮，微波功率250W，萃取温度为55℃，萃取时间为20min，制得提取液。将提取液进行抽滤，获得滤液，将滤液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出丙酮可重复利用。将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂。计算磷酸三苯酯提取率分别为90.99%、92.96%、91.79%（图4）。
比较例1
取1g样品置于索式提取装置中，加入60mL丙酮，提取温度为60℃，提取时间为480min，制得提取液；将提取液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出丙酮可重复利用。将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂；计算磷酸三苯酯提取率为70.4%。
比较例2
取1g样品、50mL丙酮置于圆底烧瓶后放入超声提取装置中，提取时间为60min，制得提取液；将提取液进行抽滤，获得滤液，将滤液旋转蒸发（35℃）除去溶剂，制得粗产品，蒸出丙酮可重复利用。将制得的产品重新用色谱纯乙酸乙酯溶解并稀释，利用气相色谱法-质谱法联用测定稀释10000倍后的磷系阻燃剂。计算磷酸三苯酯提取率为75.52%。
以上所述仅为本发明的几种较佳实施案例，本领域技术人员在不脱离本申请原理的前提下做出的若干改进和优化，也应视为本申请的保护范围。
Claims (1)
1.一种微波辅助萃取偏光膜中环保型无卤阻燃剂的方法，其特征在于，包括如下步骤：
1）将人工拆解废弃液晶面板得到废弃偏光膜进行破碎，过5~100目筛后置于封口袋中备用；
2）取适量样品置于四颈圆底烧瓶后放入微波萃取仪中，加入丙酮，料液比1:50g·mL-1，微波功率250W，萃取温度为55℃，萃取时间为30min，制得提取液；其中：萃取溶剂体积为萃取容器体积的1/3-2/3；
3）将提取液进行抽滤，获得滤液，将滤液旋转蒸发除去溶剂，制得产品；其中，旋转蒸发温度为35~50℃。
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