CN114705516A - 一种再生塑料的杂质含量测定方法及其应用 - Google Patents
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Abstract
本发明公开了一种再生塑料的杂质含量测定方法,包括样品前处理,样品检测,杂质分析,生成定量估算模型。本发明的再生塑料的杂质含量测定方法,将物理检测与化学仪器检测进行结合,不仅可以分析检测再生塑料中表观可见的杂质含量还可以分析检测不可见的杂质含量。本发明不仅对再生塑料中杂质含量进行定性分析,还进行定量分析,可以大体了解同一种再生塑料中的杂质成分与含量,可以根据再生塑料的杂质分析结果生成杂质定量估算模型,对同种再生塑料样品的杂质含量进行预估。
Description
技术领域
本发明涉及一种再生塑料的杂质含量测定方法及其应用,主要应用于再生塑料的杂质成分及定量分析领域。
背景技术
塑料是重要的有机合成高分子材料,自二十世纪问世以来就以其质量轻便,加工容易,外形美观,经济实用的优点受到人们的广泛欢迎,其广泛应用于农业生产,工业加工以及人们生活的各个方面,但是随着塑料的广泛应用,塑料难以降解的缺陷也逐渐被人类重视,白色污染越来越影响人们的生活,为了减少白色污染,保护环境,对塑料制品进行回收再生产是减少塑料污染的一种良好的方式。
对塑料制品进行回收再生产,制备得到的再生塑料中由于回收原料的不纯,回收塑料中的助剂,塑化剂在回收过程中受光照,氧气,热,机械力等外界因素的影响发生氧化,发生不可逆转的化学变化,在再生产的过程中需要除去,但是仍然有少部分的杂质存留在再生塑料中,再生塑料重新应用于生产生活之前需要对其进行杂质检测,现有的检测技术只是针对再生塑料的表观可见杂质进行分析检测,对于某些不带颜色的杂质难以进行区分检测。因此本申请发明了一种再生塑料的杂质检测方法,不仅可以对表观可见的杂质进行分析,还可以实现对无色杂质的分析检测。
发明内容
为了实现对再生塑料中有色杂质和无色杂质的共同分析,本发明的第一个方面提供了一种再生塑料的杂质含量测定方法,包括样品前处理,样品检测,杂质分析,生成定量估算模型。
作为一种优选的实施方式,所述样品前处理包括待测样品的称取,待测样品的制备,制备样品的优化处理。
作为一种优选的实施方式,所述样品的称取,称取的质量为50-100mg。
作为一种优选的实施方式,所述制备样品的优化处理是将待测样品制备成厚度为4.5-13μm,直径为95-135μm的压片。
作为一种优选的实施方式,所述的样品检测选自红外光谱检测、拉曼光谱检测、差示扫描量热法检测、热重法检测、高效液相色谱法检测、气相色谱法检测、电子显微镜检测中的一种或几种的组合。
作为一种优选的实施方式,所述的杂质分析包括杂质组分的分析,杂质的定量分析。
作为一种优选的实施方式,所述杂质的定量分析公式为:W=S杂质/S再生塑料。
作为一种优选的实施方式,所述杂质组分的分析至少包括对酯,酮,醚,酸,过酸,过酯类氧化物的分析。
作为一种优选的实施方式,所述生成定量估算模型为依据样品中不同杂质的含量制定样品杂质含量评估模型,可以对类似样品的杂质含量进行预测。
本发明的第二个方面提供了一种再生塑料的杂质含量测定方法的应用,至少应用于再生塑料PP,ABS,PVC,PA,PC,PS,PE,聚酯的杂质含量测定中。与现有技术相比,本发明具有以下有益效果:
(1)本发明的再生塑料的杂质含量测定方法,将物理检测与化学仪器检测进行结合,不仅可以分析检测再生塑料中表观可见的杂质含量还可以分析检测不可见的杂质含量。
(2)本发明的再生塑料的杂质含量测定方法,对样品进行优化前处理,通过制备标准化膜片可以将再生塑料分成均匀的样品,使每一份样品的杂质含量差距不会太大,减小了测量偏差。
(3)本发明的再生塑料的杂质含量测定方法,不仅对样品进行定性分析,还进行定量化处理,可以大体了解同一种再生塑料中的杂质成分与含量。
(4)本发明的再生塑料的杂质含量测定方法,可以根据再生塑料的杂质分析结果生成杂质定量估算模型,对同种再生塑料样品的杂质含量检测进行预估。
具体实施方式
为了实现对再生塑料中有色杂质和无色杂质的共同分析,本发明的第一个方面提供了一种再生塑料的杂质含量测定方法,包括样品前处理,样品检测,杂质分析,生成定量估算模型。
作为一种优选的实施方式,所述样品前处理包括待测样品的称取,待测样品的制备,制备样品的优化处理。
作为一种优选的实施方式,所述样品的称取,称取的质量为50-100mg。
作为一种优选的实施方式,所述样品的制备,方法为:取待测再生塑料50-100mg,将再生塑料投入平板硫化机中,采用15-20Mpa的压力压榨1-5min。
作为一种优选的实施方式,所述制备样品的优化处理是将待测样品制备成厚度为4.5-13μm,直径为95-135μm的压片。
作为一种优选的实施方式,所述的样品检测选自红外光谱检测、拉曼光谱检测、差示扫描量热法检测、热重法检测、高效液相色谱法检测、气相色谱法检测、电子显微镜检测中的一种或几种的组合。
作为一种优选的实施方式,所述的样品检测为红外光谱检测,差示扫描量热法检测,电子显微镜检测的组合。
进一步优选,红外光谱检测的检测波长范围为0.75-25μm。
进一步优选,差示扫描量热法检测中,自室温以10-15℃/min的升温速率升温至210-230℃,恒温1-3min,再以10-15℃/min的降温速率降温至170-190℃,恒温20-40min,再以10-15℃/min的降温速率降温至120-150℃,恒温20-40min。
作为一种优选的实施方式,在电子显微镜检测中,异色杂质直径≤0.1μm计1分,异色杂质≤0.5μm计3份,异色杂质≤1μm计6分。
作为一种优选的实施方式,所述的杂质分析包括杂质组分的分析,杂质的定量分析。
作为一种优选的实施方式,所述杂质的定量分析公式为:W=S杂质/S再生塑料。
作为一种优选的实施方式,所述杂质组分的分析至少包括对酯,酮,醚,酸,过酸,过酯类氧化物的分析。
作为一种优选的实施方式,所述生成定量估算模型为依据样品中不同杂质的含量制定样品杂质含量评估模型,可以对类似样品的杂质含量进行预测。
本发明的第二个方面提供了一种再生塑料的杂质含量测定方法的应用,至少应用于再生塑料PP,ABS,PVC,PA,PC,PS,PE,聚酯的杂质含量测定中。
本申请人发现再生塑料因为氧化反应会使材料的含氧量升高,生成大量酯,酮,醚,酸,过酸,过酯类氧化物,对于有机基团可以采用红外光谱检测的方式,傅里叶红外光谱仪给出不同基团的结构信息,通过比较标准谱图的峰面积与测试样品的峰面积,区分出杂质的峰,并且根据杂质峰的峰面积进行定量。
结晶度可以表示材料的降解程度,再生塑料在降解过程中产生的断链会增大材料的结晶度,而氧化产物类的杂质可能会影响重结晶,对于含有杂质的再生塑料可能会存在不均匀的晶型结构。含有杂质的样品进行差示扫描量热法进行检测时会出现多重峰,而不含杂质的再生塑料的样品进行检测时出现的熔融峰相对较简单。利用梯度等温结晶法对样品进行预处理,并按照预设的升温程序进行测试,分别得到各样品的熔融曲线。将含有杂质的样品与不含杂质样品的熔融峰曲线进行对照,并根据熔融峰的峰面积将杂质含量进行量化,根据杂质含量的计算公式W=S杂质/S再生塑料计算得出杂质在整体再生塑料中的含量比值。
对于再生塑料中的异色杂质可以通过扫描电子显微镜或者透射电子显微镜进行外观检测,比如透明材料中或者白色材料中的黑色杂质。将再生塑料材料中的异色杂质根据异色杂质的直径或者面积大小进行等级划分,直径或者面积越大的杂质等级分数越高,异色杂质直径≤0.1μm计1分,异色杂质≤0.5μm计3分,异色杂质≤1μm计6分,一个再生塑料样品中异色杂质的等级得分越高说明该再生塑料样品的杂质含量越高。并且在一个样品中若出现两个及以上的异色杂质,则会对异色杂质等级得分进行累计,计算最终再生塑料样品的等级得分。
下面通过实施例对本发明进行具体描述。有必要在此指出的是,以下实施例只用于对本发明作进一步说明,不能理解为对本发明保护范围的限制,该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整,仍属于本发明的保护范围。
实施例1
一种再生塑料的杂质含量测定方法,首先进行样品前处理,称取75mg的再生聚丙烯塑料,将其投入硫化机中进行压片,20Mpa压力下压制2min,所制得的压片的厚度为9μm,直径为100μm。将制得的样品压片放入扫描电子显微镜中进行扫描检测,对样品压片中的异色杂质进行等级评判,计算样品压片的异色杂质等级得分。
将制得的样品压片放入傅里叶变幻红外光谱仪中扫描红外谱图,扫描在0.75~25μm波长下的红外谱图,将样品的红外谱图与再生塑料的标准红外谱图进行对照,比对出样品中含有的杂质成分,并根据杂质峰的峰面积大小进行定量计算。
将制备的样品压片放到专用铝制样品盘中,做密封压盖处理,将标准再生塑料与测试样品放入差示扫描量热仪中,以梯度等温结晶法检测样品,以15℃/min的升温速率升温至230℃,恒温2分钟,再以15℃/min的降温速率降温至180℃,恒温30min,再以15℃/min的降温速率降温至150℃,恒温30min。分别得到标准再生塑料和测试样品的熔融曲线。根据公式W=S杂质/S再生塑料定量计算杂质含量。
根据再生聚丙烯塑料的杂质含量测定结果生成再生聚丙烯塑料杂质定量估算模型,有针对性的对再生聚丙烯塑料的杂质含量进行估算。不同原料来源的再生塑料中含有的杂质种类和数量大体一致,将不同原料来源的再生塑料中的杂质生成多条不同的杂质种类-杂质数量曲线,针对具体种类的再生塑料对应相应的曲线,得到杂质的预估信息,然后有针对性的选择测试方法。
Claims (10)
1.一种再生塑料的杂质含量测定方法,其特征在于,包括样品前处理,样品检测,杂质分析,生成定量估算模型。
2.根据权利要求1所述的再生塑料的杂质含量测定方法,其特征在于,所述样品前处理包括待测样品的称取,待测样品的制备,制备样品的优化处理。
3.根据权利要求2所述的再生塑料的杂质含量测定方法,其特征在于,所述样品的称取,称取的质量为50-100mg。
4.根据权利要求2所述的再生塑料的杂质含量测定方法,其特征在于,所述制备样品的优化处理是将待测样品制备成厚度为4.5-13μm,直径为95-135μm的压片。
5.根据权利要求1所述的再生塑料的杂质含量测定方法,其特征在于,所述的样品检测选自红外光谱检测、拉曼光谱检测、差示扫描量热法检测、热重法检测、高效液相色谱法检测、气相色谱法检测、电子显微镜检测中的一种或几种的组合。
6.根据权利要求1所述的再生塑料的杂质含量测定方法,其特征在于,所述的杂质分析包括杂质组分的分析,杂质的定量分析。
7.根据权利要求6所述的再生塑料的杂质含量测定方法,其特征在于,所述杂质的定量分析公式为:W=S杂质/S再生塑料。
8.根据权利要求6所述的再生塑料的杂质含量测定方法,其特征在于,所述杂质组分的分析至少包括对酯,酮,醚,酸,过酸,过酯类氧化物的分析。
9.根据权利要求1所述的再生塑料的杂质含量测定方法,其特征在于,所述生成定量估算模型为依据样品中不同杂质的含量制定样品杂质含量评估模型。
10.一种根据权利要求1-9任一项所述的再生塑料的杂质含量测定方法的应用,其特征在于,至少应用于再生塑料PP,ABS,PVC,PA,PC,PS,PE,聚酯的杂质含量测定中。
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