几种复杂塑料助剂的综合剖析研究
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摘要
为了促进我国四个现代化建设,引进国内外先进科学技术是一条重要的途径。对国外新产品进行剖析,就是引进国外先进技术的重要来源之一,也是直接取得第一手国外先进技术资料的途径之一。有关国外新产品的组成配比资料一般是文献上,甚至专利上也很难找到的。所以从某种意义上说,剖析工作是高速度发展我国材料工业、扩大材料应用的侦察兵。
本研究是利用现代分析手段对几种塑料助剂(表面改性剂、无机填料、ACR等)进行的综合剖析工作。
1.研究了一种无机填料表面改性剂的分离纯化和成分分析过程,利用红外光谱和气相色谱-质谱对表面改性剂成分进行了定性和定量分析。未知表面改性剂用正己烷和三氯甲烷溶解后,过滤分离,滤液部分用HP-5MS毛细管色谱柱检测;柱温从70℃开始,以20℃/min程序升温至260℃,保持40分钟;采用全扫描(SCN)方式;采用峰面积归一化法,计算出这些化合物的相对含量。根据实验数据确定其滤液部分共含有22中有机化合物,且其主要成分是棕榈酸和硬脂酸。滤渣部分用红外光谱测定其成分为氧化聚乙烯蜡。经过定量分析可知,氧化聚乙烯蜡的含量为53.6%;棕榈酸的含量为22.5%;硬脂酸的含量为10.5%。
2.本研究对改性后的无机填料进行了分离纯化和成分分析,并对无机填料粒径的大小进行了测试。利用红外光谱仪、气相色谱/质谱联用仪、ICP-MS和粒径分析仪对该无机填料进行了综合剖析。根据实验数据确定:该无机填料的主要成分是二氧化硅;无机填料的表面改性剂的成分是铝钛复合偶联剂;该无机填料的平均粒径大小为21.09μm,其中10μm-30μm的约占62%。
3.本研究对ACR进行了分离纯化和成分分析。利用红外光谱仪、气相色谱/质谱联用仪对该产品进行了综合剖析。共鉴定出12种化合物,其中的无机填料是碳酸钙;有机化合物中的主要成分是脂肪酸酯类。
Fetching in advanced technology of home and abroad is an important way for accelerating development of our country. The analysis for overseas new product is one of the important quarries for bringing in overseas advanced technology and that is one of ways for gaining firsthand overseas advanced technology data. It is difficulty that discovering the composing and rate of overseas new product in commonly literatures even patent. In a sense, the analysis is scout for high-speed development of China's industrial materials and expanding the application of material.
In this paper, all-around analyses of several plastic additives (surface modifiers; inorganic filler; ACR et al.) have been completed, and quantitative analyses of the major components also have been completed.
1. The separation and the analytical process for clarifieation of the composition of an unknown surface modification additive was reported in this paper; Qualitative analysis and quantitative analysis of the surface modification additive were completed by using infrared spectrometry and GC-MS. A unknow surface modification additive was solved by n-hexane and chloroform, and separation was completed by using filtration. The filtrate was determined by GC-MS with HP-5MS capillary column in the scan monitoring mode. Column temperature gradient: initial temperature 70℃, and then increased at 20℃/ min to 260℃, and maintain 40min. SCN is collection method. We calculated the relative amount of these compounds by using peak area normalization method. According to the experimental data, the liquid part contains 22 organic compounds. The content of palm acid is the highest, next stearic acid. The residue was determined by infrared spectrometry and the component is oxidation polyethylene. Through quantitative analysis, we can see that the content of oxidation polyethylene is 53.6%. The content of palm acid is 22.5%, and the content of stearic acid is 10.5%.
2. In this study, the separation and the analytical process for the activation inorganic filler have been completed, and the size of particle has been tested. We completed the all-around analyses of the inorganic filler by using infrared spectroscopy, GC-MS, ICP-MS and particle size analyzer. Its main ingredient is silica. Component of surface modification is titanium aluminum compound coupling agent. The average particle size of inorganic filler is 21.09μm, in which 10μm-30μm is about 62%
3. In this study, the separation and the analytical process for ACR have been completed. Infrared spectroscopy and GC-MS were used for completing the analysis of ACR. 12 kinds of compounds were identified, in which the inorganic filler is calcium carbonate and organic compounds is the main ingredient in fatty acid esters.
本研究是利用现代分析手段对几种塑料助剂(表面改性剂、无机填料、ACR等)进行的综合剖析工作。
1.研究了一种无机填料表面改性剂的分离纯化和成分分析过程,利用红外光谱和气相色谱-质谱对表面改性剂成分进行了定性和定量分析。未知表面改性剂用正己烷和三氯甲烷溶解后,过滤分离,滤液部分用HP-5MS毛细管色谱柱检测;柱温从70℃开始,以20℃/min程序升温至260℃,保持40分钟;采用全扫描(SCN)方式;采用峰面积归一化法,计算出这些化合物的相对含量。根据实验数据确定其滤液部分共含有22中有机化合物,且其主要成分是棕榈酸和硬脂酸。滤渣部分用红外光谱测定其成分为氧化聚乙烯蜡。经过定量分析可知,氧化聚乙烯蜡的含量为53.6%;棕榈酸的含量为22.5%;硬脂酸的含量为10.5%。
2.本研究对改性后的无机填料进行了分离纯化和成分分析,并对无机填料粒径的大小进行了测试。利用红外光谱仪、气相色谱/质谱联用仪、ICP-MS和粒径分析仪对该无机填料进行了综合剖析。根据实验数据确定:该无机填料的主要成分是二氧化硅;无机填料的表面改性剂的成分是铝钛复合偶联剂;该无机填料的平均粒径大小为21.09μm,其中10μm-30μm的约占62%。
3.本研究对ACR进行了分离纯化和成分分析。利用红外光谱仪、气相色谱/质谱联用仪对该产品进行了综合剖析。共鉴定出12种化合物,其中的无机填料是碳酸钙;有机化合物中的主要成分是脂肪酸酯类。
Fetching in advanced technology of home and abroad is an important way for accelerating development of our country. The analysis for overseas new product is one of the important quarries for bringing in overseas advanced technology and that is one of ways for gaining firsthand overseas advanced technology data. It is difficulty that discovering the composing and rate of overseas new product in commonly literatures even patent. In a sense, the analysis is scout for high-speed development of China's industrial materials and expanding the application of material.
In this paper, all-around analyses of several plastic additives (surface modifiers; inorganic filler; ACR et al.) have been completed, and quantitative analyses of the major components also have been completed.
1. The separation and the analytical process for clarifieation of the composition of an unknown surface modification additive was reported in this paper; Qualitative analysis and quantitative analysis of the surface modification additive were completed by using infrared spectrometry and GC-MS. A unknow surface modification additive was solved by n-hexane and chloroform, and separation was completed by using filtration. The filtrate was determined by GC-MS with HP-5MS capillary column in the scan monitoring mode. Column temperature gradient: initial temperature 70℃, and then increased at 20℃/ min to 260℃, and maintain 40min. SCN is collection method. We calculated the relative amount of these compounds by using peak area normalization method. According to the experimental data, the liquid part contains 22 organic compounds. The content of palm acid is the highest, next stearic acid. The residue was determined by infrared spectrometry and the component is oxidation polyethylene. Through quantitative analysis, we can see that the content of oxidation polyethylene is 53.6%. The content of palm acid is 22.5%, and the content of stearic acid is 10.5%.
2. In this study, the separation and the analytical process for the activation inorganic filler have been completed, and the size of particle has been tested. We completed the all-around analyses of the inorganic filler by using infrared spectroscopy, GC-MS, ICP-MS and particle size analyzer. Its main ingredient is silica. Component of surface modification is titanium aluminum compound coupling agent. The average particle size of inorganic filler is 21.09μm, in which 10μm-30μm is about 62%
3. In this study, the separation and the analytical process for ACR have been completed. Infrared spectroscopy and GC-MS were used for completing the analysis of ACR. 12 kinds of compounds were identified, in which the inorganic filler is calcium carbonate and organic compounds is the main ingredient in fatty acid esters.
引文
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[10] 郑宁来.PVC 助剂的新进展[J].塑料助剂,2004(3):1-3.
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