超支化共聚物复鞣填充剂的制备及应用
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摘要
三羟甲基丙烷与顺丁烯二酸酐通过酯化反应合成了超支化中间体单酯,以三羟甲基丙烷顺丁烯二酸单酯和甲基丙烯酸(MAA)作单体,通过自由基聚合制备了超支化马来酸单酯-甲基丙烯酸共聚物(HCPMM),将其用于皮革复鞣。
马来酸酐与三羟甲基丙烷通过酯化反应合成超支化中间体(MTP)。通过测定酸值跟踪反应的历程,考察了分散介质、催化剂用量、醇酐摩尔用量比、反应时间、反应温度等因素对酯化反应的影响。用红外光谱(FTIR)和核磁共振(NMR)表征超支化中间体的结构。
通过自由基聚合制备超支化马来酸酐衍生物-甲基丙烯酸共聚物,考察了MTP类型、原料配比、引发剂用量、反应温度、反应时间等合成工艺对反应的影响。用红外光谱和核磁共振表征产物的结构,通过凝胶渗透色谱仪(GPC)测定HPCMM的相对分子质量。结果表明聚合体系较佳的合成工艺为：选用MTP-25为超支化中间体,MTP-25与甲基丙烯酸(MAA)的摩尔比为1：6,引发剂用量为反应单体的4%,聚合温度控制在80℃,反应时间为4-5h。HPCMM的相对分子质量为3160g/mol,热稳定性一般。
将HPCMM复鞣填充剂用于绵羊蓝湿服装革的复鞣,通过考察皮革填充性、柔软性等性能指标,探索复鞣填充剂的最佳应用工艺。研究结果表明：该复鞣剂有很明显的填充作用,与染料、油脂的协同作用好；经HPCMM复鞣剂复鞣后的坯革柔软、丰满、有弹性、表面着色均匀,物理机械强度稍有下降。
The synthesis of hyperbranched coploymaleate-methacrylic (HPCMM) by radical polymerization with methacrylic acid and maleate-methacrylic as monomers was detailedly studied. Excellent properties were found when the HPCMM was used in retanning progress of leather making.
Based on trimethylol propane and maleic anhydride as raw material, mono-esterification product was synthesized as the hyperbranched intermediates. The reactive couse was tracking with testing acid value. The influences of solvent, catalyst, molar ratio between trimethylol propane and maleic anhydride, time and temperature were studied. The characteristics of the hyperbranched intermediates were determined by Fourier transform infrared (FTIR) and nuclear magnetic resonance spectroscopy (NMR).
HPCMM was synthesized by radical polymerization, and then the influences of types of MTP, molar ratio between MTP and methacrylic, initiator dosage, the reaction temperature and time were discussed. The characteristics of HPCMM were determined by FTIR and NMR. The molecular weight was surveyed by Gel Permeation Chromatograph (GPC). The results showed that the optimum reaction conditions were the type of hyperbranched intermediates was used MTP-25; molar ratio between MTP and methacrylic was 1:6; initiator dosage was 4% of monomers; the reaction time was about 4h; the reaction temperature was 80℃. The molecular weight of HPCMM was 3160g/mol. Sthermal stability of HPCMM was nothing special.
A retanning and filling agent HPCMM was applied in the retanning of chrome-tanned sheep garment leather. According to the research of indexes such as filling quality and pliability, the optimum retanning parameters were discussed in detail. The results showed that the retanning agent could fill leather to a certain degree, had good synergistic effect with dyestuff and oil, the sheep garment leather retanned with HPCMM was soft, full and elastic and possesses good color effect, while its physical properties was lightly declined.
马来酸酐与三羟甲基丙烷通过酯化反应合成超支化中间体(MTP)。通过测定酸值跟踪反应的历程,考察了分散介质、催化剂用量、醇酐摩尔用量比、反应时间、反应温度等因素对酯化反应的影响。用红外光谱(FTIR)和核磁共振(NMR)表征超支化中间体的结构。
通过自由基聚合制备超支化马来酸酐衍生物-甲基丙烯酸共聚物,考察了MTP类型、原料配比、引发剂用量、反应温度、反应时间等合成工艺对反应的影响。用红外光谱和核磁共振表征产物的结构,通过凝胶渗透色谱仪(GPC)测定HPCMM的相对分子质量。结果表明聚合体系较佳的合成工艺为：选用MTP-25为超支化中间体,MTP-25与甲基丙烯酸(MAA)的摩尔比为1：6,引发剂用量为反应单体的4%,聚合温度控制在80℃,反应时间为4-5h。HPCMM的相对分子质量为3160g/mol,热稳定性一般。
将HPCMM复鞣填充剂用于绵羊蓝湿服装革的复鞣,通过考察皮革填充性、柔软性等性能指标,探索复鞣填充剂的最佳应用工艺。研究结果表明：该复鞣剂有很明显的填充作用,与染料、油脂的协同作用好；经HPCMM复鞣剂复鞣后的坯革柔软、丰满、有弹性、表面着色均匀,物理机械强度稍有下降。
The synthesis of hyperbranched coploymaleate-methacrylic (HPCMM) by radical polymerization with methacrylic acid and maleate-methacrylic as monomers was detailedly studied. Excellent properties were found when the HPCMM was used in retanning progress of leather making.
Based on trimethylol propane and maleic anhydride as raw material, mono-esterification product was synthesized as the hyperbranched intermediates. The reactive couse was tracking with testing acid value. The influences of solvent, catalyst, molar ratio between trimethylol propane and maleic anhydride, time and temperature were studied. The characteristics of the hyperbranched intermediates were determined by Fourier transform infrared (FTIR) and nuclear magnetic resonance spectroscopy (NMR).
HPCMM was synthesized by radical polymerization, and then the influences of types of MTP, molar ratio between MTP and methacrylic, initiator dosage, the reaction temperature and time were discussed. The characteristics of HPCMM were determined by FTIR and NMR. The molecular weight was surveyed by Gel Permeation Chromatograph (GPC). The results showed that the optimum reaction conditions were the type of hyperbranched intermediates was used MTP-25; molar ratio between MTP and methacrylic was 1:6; initiator dosage was 4% of monomers; the reaction time was about 4h; the reaction temperature was 80℃. The molecular weight of HPCMM was 3160g/mol. Sthermal stability of HPCMM was nothing special.
A retanning and filling agent HPCMM was applied in the retanning of chrome-tanned sheep garment leather. According to the research of indexes such as filling quality and pliability, the optimum retanning parameters were discussed in detail. The results showed that the retanning agent could fill leather to a certain degree, had good synergistic effect with dyestuff and oil, the sheep garment leather retanned with HPCMM was soft, full and elastic and possesses good color effect, while its physical properties was lightly declined.
引文
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