纸塑复合包装材料UV墨光引发剂迁移试验与理论研究
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摘要
紫外光(Ultraviolet,简称UV)固化墨以其本身的优异特性被广泛用于食品包装印刷,虽然它不存在溶剂挥发问题,但是所用的低分子量光引发剂具有一定毒性,对皮肤有一定的刺激性,而且容易挥发和迁移,给被包装食品带来难闻气味,甚至毒性,对人体健康是一种威胁。
论文就纸塑复合包装材料纸中助剂及光引发剂的检测技术、光引发剂迁移试验及理论迁移预测模型的建立进行了系统性的研究,主要内容包括以下几个方面:
1. GC-FID(gas chromatography-flame ionization detection气相色谱-氢火焰离子化检测器)检测方法的确立
研究确定UV墨中光引发剂α-羟基环己基苯基甲酮(184)和2,2-二甲氧基-苯基甲酮(651)标准品GC-FID检测条件;
研究确定纸塑复合包装材料纸中助剂、光引发剂184和651的GC-FID检测条件:HP-5毛细管柱,检测器温度250℃,进样口温度250℃,不分流进样,进样量1μL,载气为氮气,升温程序:初始温度100℃,以5℃/min升至200℃,保持2min,再以35℃/min升至300℃,保持5min。
2. UV墨光引发剂稳定性试验研究
试验研究了20℃、40℃和60℃温度条件下184和651在10%、95%乙醇水溶液和异辛烷中的避光稳定性,同时考察了光稳定剂对羟基苯甲醚(HQMME)的加入在避光条件下对稳定性的影响。结果表明,避光条件下,光稳定剂对184和651的稳定性影响不显著;除60℃温度条件下651在10%乙醇水溶液中存在不稳定外,其它条件下184和651都是稳定的;利用GC-MS对651的分解产物进行了定性分析。
3.纸塑复合包装材料纸中光引发剂的迁移试验研究
试验研究了20℃、40℃和60℃温度条件下,纸塑复合材料4015、6515中184和651向10%、95%乙醇和异辛烷的迁移;材料4025中184和651向10%乙醇和异辛烷的迁移;材料3312中184和651向95%乙醇和异辛烷的迁移。结果表明,同一污染物向同一食品模拟物的迁移受温度影响显著;在同样的试验条件下分子量大的651的迁移速率低于分子量小的184的迁移速率;同一污染物在同一试验温度下向异辛烷中的迁移速度最快,向10%乙醇水溶液中的迁移速度最慢;随着低密度聚乙烯(low density polyethylene,LDPE)淋膜量的加大,迁移量明显减少;聚丙烯(polypropylene, PP)的阻隔特性优于LDPE的阻隔特性;同种试验条件下,松厚度大的纸中污染物的迁移速度相对较快;迁移量随污染物初始浓度的增大明显增大。文中还从“微观”角度分析了温度、污染物分子结构、食品模拟物的溶胀、淋膜层厚度、淋膜层种类和纸张性质对迁移的影响。
4.迁移预测模型的建立
建立了无限厚纸层迁移预测模型和有限厚纸层迁移预测模型,模型分别将纸的厚度作为无限厚(相对于塑料涂层厚度)和有限厚进行考虑,包装食品体系作为有限包装-无限食品进行研究。模型引入新的参量纸和塑料界面处的分配系数kCP、考虑了污染物在纸和塑料涂层中不同的扩散系数DP、DC,最终给出扩散方程、初始条件和边界条件,用拉普拉斯和反拉普拉斯变换对方程求一系列解析解,并分析了各参量kCP、DP、DC和纸中污染物初始浓度CP0等对迁移行为的影响。
5.有限厚纸层迁移预测模型通用性及与实验值的对比分析
讨论了有限厚纸层迁移预测模型简化后作为双层复合塑料和单层塑料中污染物向食品中迁移的预测模型通用性。简化的双层塑料预测模型表达式最终与著名的Laoubi-Vergnaud模型一致,简化的单层塑料预测模型最终为著名的Crank迁移扩散表达式。
根据试验测定的纸塑界面处分配系数及结合其它参数,将不同纸塑复合包装材料中污染物184和651向不同食品模拟物的迁移实验值与有限厚纸层迁移模型预测值进行了对比,得出结论:当预测模型中采用的污染物在塑料涂层中的扩散系数为高估扩散系数时,预测模型能最大限度的保证包装的使用安全性。另外,得出结论:无限厚纸层迁移预测模型不适合纸厚度较薄的纸塑复合包装材料中污染物向食品(或食品模拟物)中迁移量的预测。
Ultraviolet (UV) inks are widely used in food-packaging printing due to their excellent properties. They generally do not contain any traditional organic solvents. However, photoinitiators (PIs) are known to give taints, odors, potential migration problems or are suspected to give rise to toxicological problems, which would be a health hazards to consumers.
In this paper, detection techniques of additives and PIs, migration experiment and mathematical modeling of migration of PIs from paper-plastic coating materials into food were discussed. The contents are as followings.
1. Research on the detection methods of GC-FID (gas chromatography-flame ionization detection)
The GC-FID detection method for the standard of UV ink PIs
1-hydroxycyclohexyl-1-phenyl ketone (184) and Benzyldimethyl ketal (651) was built. The GC-FID detection method for the analysed 184, 651 and additives from paper-plastic coating materials was built, the detection conditions were as followings: a HP-5 capillary column. Temperature programme set at 100℃initially, then increased by 5℃/min up to 200℃, with a holding time of 2min, then increased by 35℃/min up to 300℃, with a holding time of 5min. Injection volume was 1μL and carrier gas was nitrogen at 2.5mL/min. The injector and detector temperature were 250℃, respectively. The injection was made in a splitless mode.
2. Study on the stability of UV ink PIs
Stability of 184 and 651 in 10%, 95% ethanol and isooctane at 20℃, 40℃and 60℃was studied under no light exposure. At the same time, the effect of stabilizing agent hydroquinone monomethyl ester (HQMME) on stability was discussed. The results showed that the effect of protection of HQMME was not obvious under all heat-exposure conditions tested and in all food simulants used under no light exposure conditions. Photoinitiator 184 was shown to be quite stable under all heat-exposure conditions tested and in all food simulants used whether adding HQMME or not. Photoinitiator 651 was stable almost in all heat-exposure conditions tested and in all food simulants used except in food simulant 10% ethanol at 60℃. The mass spectrum of decomposed product of 651 was detected by GC-MS.
3. Study on migration of PIs from paper-plastic coating materials
Migration of 184 and 651 from paper-plastic coating materials 4015 and 6515 into 10%, 95% ethanol and isooctane, from 4025 into 10% ethanol and isooctane, from 3312 into 95% ethanol and isooctane at 20℃, 40℃and 60℃were studied. The results showed that the effect of temperature on migration of the same contaminant into the same food stimulant was obvious. The diffusion rate of high molecular weight 651 was much lower than that of low molecular weight 184. Migration rate of the same contaminant into isooctane was the fastest. However, migration rate into 10% ethanol was the lowest at the same test conditions. The migration amount decreased with the increase of LDPE thickness. The barrier property of PP was better than that of LDPE. At the same test conditions, migration rate of contaminant was relatively slow from high tightness paper. It was also showed that migration amount increased with the increase of initial concentration of contaminant. In addition, the effect factors on migration were also analyzed from a microcosmic viewpoint. The factors included temperature, molecular structure of contaminant, swelling of food simulants, thickness of plastic coating, type of plastic coating and property of paper.
4. Migration modeling
Migration mathematical modeling of unlimited paper thickness and limited paper thickness were built. In the two modelings, the thickness of paper was considered as unlimited thickness (as far as the thickness of plastic coating was considered) and as limited thickness, respectively. Packaging-food system was studied as limited packaging-unlimited food. New parameter of partition coefficient at the interface of paper and plastic coating was introduced, different diffusion coefficients DP and DC of contaminant in paper and plastic coating were considered. In addition, diffusion equations, initial conditions and boundary conditions were given. A series of analytical solutions were obtained through Laplace transformation and inversion theorem. The effect of kCP, DP, DC and initial concentration CP0, et al on migration behavior was discussed.
5. Applicability of mathematical modeling of limited paper thickness and contrastive analysis with experiment values
The applicability of mathematical modeling of limited paper thickness as bi-layer polymer packaging and mono-layer polymer packaging was studied. The expression of simplified bi-layer polymer was accordant with the famous Laoubi-Vergnaud modeling, and the expression of simplified mono-layer polymer was the famous Crank diffusion modeling.
According to experimental values of partition coefficient kCP at paper-plastic interface and combining other parameters, migration experiment values of PIs 184 and 651 from different paper-plastic materials into different food simulants and calculated values from limited paper thickness modeling were compared. It showed the results that this mathematical modeling with the“worst-case”Dc could ensure the using safety of packaging. In addition, migration mathematical modeling of unlimited paper thickness was not appropriate to predict the migration of contaminants into food or food simulants from paper-plastic materials with thiner paper thickness.
论文就纸塑复合包装材料纸中助剂及光引发剂的检测技术、光引发剂迁移试验及理论迁移预测模型的建立进行了系统性的研究,主要内容包括以下几个方面:
1. GC-FID(gas chromatography-flame ionization detection气相色谱-氢火焰离子化检测器)检测方法的确立
研究确定UV墨中光引发剂α-羟基环己基苯基甲酮(184)和2,2-二甲氧基-苯基甲酮(651)标准品GC-FID检测条件;
研究确定纸塑复合包装材料纸中助剂、光引发剂184和651的GC-FID检测条件:HP-5毛细管柱,检测器温度250℃,进样口温度250℃,不分流进样,进样量1μL,载气为氮气,升温程序:初始温度100℃,以5℃/min升至200℃,保持2min,再以35℃/min升至300℃,保持5min。
2. UV墨光引发剂稳定性试验研究
试验研究了20℃、40℃和60℃温度条件下184和651在10%、95%乙醇水溶液和异辛烷中的避光稳定性,同时考察了光稳定剂对羟基苯甲醚(HQMME)的加入在避光条件下对稳定性的影响。结果表明,避光条件下,光稳定剂对184和651的稳定性影响不显著;除60℃温度条件下651在10%乙醇水溶液中存在不稳定外,其它条件下184和651都是稳定的;利用GC-MS对651的分解产物进行了定性分析。
3.纸塑复合包装材料纸中光引发剂的迁移试验研究
试验研究了20℃、40℃和60℃温度条件下,纸塑复合材料4015、6515中184和651向10%、95%乙醇和异辛烷的迁移;材料4025中184和651向10%乙醇和异辛烷的迁移;材料3312中184和651向95%乙醇和异辛烷的迁移。结果表明,同一污染物向同一食品模拟物的迁移受温度影响显著;在同样的试验条件下分子量大的651的迁移速率低于分子量小的184的迁移速率;同一污染物在同一试验温度下向异辛烷中的迁移速度最快,向10%乙醇水溶液中的迁移速度最慢;随着低密度聚乙烯(low density polyethylene,LDPE)淋膜量的加大,迁移量明显减少;聚丙烯(polypropylene, PP)的阻隔特性优于LDPE的阻隔特性;同种试验条件下,松厚度大的纸中污染物的迁移速度相对较快;迁移量随污染物初始浓度的增大明显增大。文中还从“微观”角度分析了温度、污染物分子结构、食品模拟物的溶胀、淋膜层厚度、淋膜层种类和纸张性质对迁移的影响。
4.迁移预测模型的建立
建立了无限厚纸层迁移预测模型和有限厚纸层迁移预测模型,模型分别将纸的厚度作为无限厚(相对于塑料涂层厚度)和有限厚进行考虑,包装食品体系作为有限包装-无限食品进行研究。模型引入新的参量纸和塑料界面处的分配系数kCP、考虑了污染物在纸和塑料涂层中不同的扩散系数DP、DC,最终给出扩散方程、初始条件和边界条件,用拉普拉斯和反拉普拉斯变换对方程求一系列解析解,并分析了各参量kCP、DP、DC和纸中污染物初始浓度CP0等对迁移行为的影响。
5.有限厚纸层迁移预测模型通用性及与实验值的对比分析
讨论了有限厚纸层迁移预测模型简化后作为双层复合塑料和单层塑料中污染物向食品中迁移的预测模型通用性。简化的双层塑料预测模型表达式最终与著名的Laoubi-Vergnaud模型一致,简化的单层塑料预测模型最终为著名的Crank迁移扩散表达式。
根据试验测定的纸塑界面处分配系数及结合其它参数,将不同纸塑复合包装材料中污染物184和651向不同食品模拟物的迁移实验值与有限厚纸层迁移模型预测值进行了对比,得出结论:当预测模型中采用的污染物在塑料涂层中的扩散系数为高估扩散系数时,预测模型能最大限度的保证包装的使用安全性。另外,得出结论:无限厚纸层迁移预测模型不适合纸厚度较薄的纸塑复合包装材料中污染物向食品(或食品模拟物)中迁移量的预测。
Ultraviolet (UV) inks are widely used in food-packaging printing due to their excellent properties. They generally do not contain any traditional organic solvents. However, photoinitiators (PIs) are known to give taints, odors, potential migration problems or are suspected to give rise to toxicological problems, which would be a health hazards to consumers.
In this paper, detection techniques of additives and PIs, migration experiment and mathematical modeling of migration of PIs from paper-plastic coating materials into food were discussed. The contents are as followings.
1. Research on the detection methods of GC-FID (gas chromatography-flame ionization detection)
The GC-FID detection method for the standard of UV ink PIs
1-hydroxycyclohexyl-1-phenyl ketone (184) and Benzyldimethyl ketal (651) was built. The GC-FID detection method for the analysed 184, 651 and additives from paper-plastic coating materials was built, the detection conditions were as followings: a HP-5 capillary column. Temperature programme set at 100℃initially, then increased by 5℃/min up to 200℃, with a holding time of 2min, then increased by 35℃/min up to 300℃, with a holding time of 5min. Injection volume was 1μL and carrier gas was nitrogen at 2.5mL/min. The injector and detector temperature were 250℃, respectively. The injection was made in a splitless mode.
2. Study on the stability of UV ink PIs
Stability of 184 and 651 in 10%, 95% ethanol and isooctane at 20℃, 40℃and 60℃was studied under no light exposure. At the same time, the effect of stabilizing agent hydroquinone monomethyl ester (HQMME) on stability was discussed. The results showed that the effect of protection of HQMME was not obvious under all heat-exposure conditions tested and in all food simulants used under no light exposure conditions. Photoinitiator 184 was shown to be quite stable under all heat-exposure conditions tested and in all food simulants used whether adding HQMME or not. Photoinitiator 651 was stable almost in all heat-exposure conditions tested and in all food simulants used except in food simulant 10% ethanol at 60℃. The mass spectrum of decomposed product of 651 was detected by GC-MS.
3. Study on migration of PIs from paper-plastic coating materials
Migration of 184 and 651 from paper-plastic coating materials 4015 and 6515 into 10%, 95% ethanol and isooctane, from 4025 into 10% ethanol and isooctane, from 3312 into 95% ethanol and isooctane at 20℃, 40℃and 60℃were studied. The results showed that the effect of temperature on migration of the same contaminant into the same food stimulant was obvious. The diffusion rate of high molecular weight 651 was much lower than that of low molecular weight 184. Migration rate of the same contaminant into isooctane was the fastest. However, migration rate into 10% ethanol was the lowest at the same test conditions. The migration amount decreased with the increase of LDPE thickness. The barrier property of PP was better than that of LDPE. At the same test conditions, migration rate of contaminant was relatively slow from high tightness paper. It was also showed that migration amount increased with the increase of initial concentration of contaminant. In addition, the effect factors on migration were also analyzed from a microcosmic viewpoint. The factors included temperature, molecular structure of contaminant, swelling of food simulants, thickness of plastic coating, type of plastic coating and property of paper.
4. Migration modeling
Migration mathematical modeling of unlimited paper thickness and limited paper thickness were built. In the two modelings, the thickness of paper was considered as unlimited thickness (as far as the thickness of plastic coating was considered) and as limited thickness, respectively. Packaging-food system was studied as limited packaging-unlimited food. New parameter of partition coefficient at the interface of paper and plastic coating was introduced, different diffusion coefficients DP and DC of contaminant in paper and plastic coating were considered. In addition, diffusion equations, initial conditions and boundary conditions were given. A series of analytical solutions were obtained through Laplace transformation and inversion theorem. The effect of kCP, DP, DC and initial concentration CP0, et al on migration behavior was discussed.
5. Applicability of mathematical modeling of limited paper thickness and contrastive analysis with experiment values
The applicability of mathematical modeling of limited paper thickness as bi-layer polymer packaging and mono-layer polymer packaging was studied. The expression of simplified bi-layer polymer was accordant with the famous Laoubi-Vergnaud modeling, and the expression of simplified mono-layer polymer was the famous Crank diffusion modeling.
According to experimental values of partition coefficient kCP at paper-plastic interface and combining other parameters, migration experiment values of PIs 184 and 651 from different paper-plastic materials into different food simulants and calculated values from limited paper thickness modeling were compared. It showed the results that this mathematical modeling with the“worst-case”Dc could ensure the using safety of packaging. In addition, migration mathematical modeling of unlimited paper thickness was not appropriate to predict the migration of contaminants into food or food simulants from paper-plastic materials with thiner paper thickness.
引文
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