CN108794801A - 高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法 - Google Patents
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Abstract
高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,采用回收的PEN废料与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,反应结束后经过滤除去杂质即得到聚酯树脂。本发明实现了废旧PEN的回收利用,减少了废旧PEN对环境的污染;同时与传统工艺比较,材料成本降低程度到达30%以上,本方法制备的聚酯树脂具有较高的玻璃化温度,同时拥有较好的光泽、抗冲击性和优良的流平。
Description
技术领域
本发明涉及聚酯树脂制备技术领域,具体涉及一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法。
背景技术
目前,国内热固性粉末涂料主要由树脂、固化剂、颜填料、助剂等组成,主要分为纯聚酯粉末涂料和混合型粉末涂料,主要应用于家用金属家具、电器配件、五金构件等领域。混合型粉末涂料又称环氧-聚酯型热固性粉末涂料,多由芳香族羟酸(或酸酐)与多元醇经缩聚反应制成热固性饱和聚酯树脂。多元醇多采用是聚酯多元醇、乙二醇、二甘醇或是其混合物,芳香族羟酸主要是PTA(精对苯二甲酸),辅以偏苯三酸酐。由于多元酸选择的局限性,使用单一多元醇不能满足聚酯性能要求,往往需要对多种醇进行合理调配使用,以求使聚酯性能达到最佳。一般而言,为提高聚酯性能及稳定性,往往需要增加固体醇(新戊二醇)的含量,而固体醇的价格比较昂贵,也就增加了聚酯成本。尤其在气温偏高的季节及地域,对聚酯树脂玻璃化温度的要求较高,现阶段在聚酯生产环节仍以增加固体醇含量的方式进行调整,增加成本的同时效果并不能满足应用需求。
发明内容
本发明提供了一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,以解决现有技术存在的生产成本较高和玻璃化温度不理想的技术问题。
本发明解决其技术问题所采用的技术方案是:
一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,采用回收的聚萘二甲酸乙二酯PEN废料,PEN废料粉碎后与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,反应结束后经过滤除去杂质即得到聚酯树脂。
上述PEN废料需粉碎成5 mm~10mm粒径的碎料。
上述多元醇为乙二醇、二甘醇、三甘醇、新戊二醇、2-甲基-1,3-丙二醇、1,3-丙二醇、丙二醇、丁二醇、特戊二醇和三羟甲基丙烷的一种或多种。
上述多元酸为间苯二甲酸、精对苯二甲酸、硬脂酸、己二酸、马来酸、偏苯三酸酐和邻苯二甲酸酐的一种或多种。
上述多元醇加入量占PEN质量的100%~300%;醋酸锌加入量占PEN质量的 0.10%~0.25%;单丁基氧化锡占PEN质量的0.25%~0.60%;多元酸占PEN质量的300%~650%;亚磷酸酯三苯酯占PEN质量的0.3%~0.8%;偏苯三酸酐占PEN质量的15%~28%;十八十六叔胺占PEN质量的2.5%~5%。
上述醇解温度控制在230℃~255℃。
上述酯交换和酯化反应温度为190℃~250℃;酯交换和酯化反应结束条件为:取样分析酸值为 30±5mgKOH/g,粘度为 30±10cSt,粘度计测试温度为150±5℃。
上述减压缩聚反应条件为:反应釜内压力≤0.095Mpa,温度230℃~250℃;减压缩聚反应结束条件为:取样分析粘度15±10cSt,粘度计温度为200±5℃,酸值达到15±10mgKOH/g,羟值<5mgKOH/g。
上述减压缩聚反应中反应釜内压力控制在0.09 Mpa~0.095Mpa。
上述聚合度调整反应条件为:反应温度 200±5℃;聚合度调整反应结束条件为:取样分析酸值为50~55mgKOH/g,粘度为25 cSt~35cSt,粘度计温度为 200±5℃,羟值<5mgKOH/g。
本发明方法利用PEN材质类废料进行生产,实现了废旧 PEN 的回收利用,减少了废旧PEN对环境的污染,具有显著的环保效益;同时与传统工艺比较,材料成本降低程度到达30% 以上,同时本方法制备的聚酯树脂具有较高的玻璃化温度,同时拥有较好的光泽、抗冲击性、优良的流平,满足粉末涂料生产过程中对聚酯玻璃化的要求。
具体实施方式
例1
一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,采用回收的聚萘二甲酸乙二酯PEN废料,PEN废料粉碎成5 mm~10mm粒径的碎料与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,多元醇为乙二醇、二甘醇、三甘醇、新戊二醇、2-甲基-1,3- 丙二醇、1,3- 丙二醇、丙二醇、丁二醇、特戊二醇和三羟甲基丙烷的一种或多种,多元醇加入量占PEN质量的311%;醋酸锌加入量占PEN质量的 0.2%;单丁基氧化锡占PEN质量的0.5%,醇解温度控制在230℃~255℃,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,多元酸为间苯二甲酸、精对苯二甲酸、硬脂酸、己二酸、马来酸、偏苯三酸酐和邻苯二甲酸酐的一种或多种,多元酸占PEN质量的477%;亚磷酸酯三苯酯占PEN质量的0.5%,酯交换和酯化反应温度为190℃~250℃;酯交换和酯化反应结束条件为:取样分析酸值为 30±5mgKOH/g,粘度为 30±10cSt,粘度计测试温度为150±5℃,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应条件为:反应釜内压力≤0.095Mpa,温度230℃~250℃;减压缩聚反应结束条件为:取样分析粘度15±10cSt,粘度计温度为200±5℃,酸值达到15±10mgKOH/g,羟值<5mgKOH/g,减压缩聚反应中反应釜内压力控制在0.09 Mpa~0.095Mpa,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,偏苯三酸酐占PEN质量的50%;十八十六叔胺占PEN质量的4.2%,聚合度调整反应条件为:反应温度 200±5℃;聚合度调整反应结束条件为:取样分析酸值为50~55mgKOH/g,粘度为25 cSt~35cSt,粘度计温度为 200±5℃,羟值<5mgKOH/g,反应结束后经过滤除去杂质即得到聚酯树脂。
例2
一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,采用回收的聚萘二甲酸乙二酯PEN废料,PEN废料粉碎成5mm~10mm粒径的碎料与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,多元醇为乙二醇、二甘醇、三甘醇、新戊二醇、2-甲基-1,3-丙二醇、1,3-丙二醇、丙二醇、丁二醇、特戊二醇和三羟甲基丙烷的一种或多种,多元醇加入量占PEN质量的200%;醋酸锌加入量占PEN质量的 0.15%;单丁基氧化锡占PEN质量的0.3%,醇解温度控制在230℃~255℃,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,多元酸为间苯二甲酸、精对苯二甲酸、硬脂酸、己二酸、马来酸、偏苯三酸酐和邻苯二甲酸酐的一种或多种,多元酸占PEN质量的300%;亚磷酸酯三苯酯占PEN质量的0.4%,酯交换和酯化反应温度为190℃~250℃;酯交换和酯化反应结束条件为:取样分析酸值为 30±5mgKOH/g,粘度为 30±10cSt,粘度计测试温度为150±5℃,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应条件为:反应釜内压力≤0.095Mpa,温度230℃~250℃;减压缩聚反应结束条件为:取样分析粘度15±10cSt,粘度计温度为200±5℃,酸值达到15±10mgKOH/g,羟值<5mgKOH/g,减压缩聚反应中反应釜内压力控制在0.09 Mpa~0.095Mpa,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,偏苯三酸酐占PEN质量的35%;十八十六叔胺占PEN质量的3.2%,聚合度调整反应条件为:反应温度 200±5℃;聚合度调整反应结束条件为:取样分析酸值为50~55mgKOH/g,粘度为25 cSt~35cSt,粘度计温度为 200±5℃,羟值<5mgKOH/g,反应结束后经过滤除去杂质即得到聚酯树脂。
例3
一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,采用回收的聚萘二甲酸乙二酯PEN废料,PEN废料粉碎成5 mm~10mm粒径的碎料与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,多元醇为乙二醇、二甘醇、三甘醇、乙二醇、新戊二醇、2-甲基 -1,3-丙二醇、1,3- 丙二醇、丙二醇、丁二醇、特戊二醇和三羟甲基丙烷的一种或多种,多元醇加入量占PEN质量的300%;醋酸锌加入量占PEN质量的0.25%;单丁基氧化锡占PEN质量的0.60%,醇解温度控制在230℃~255℃,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,多元酸为间苯二甲酸、精对苯二甲酸、硬脂酸、己二酸、马来酸、偏苯三酸酐和邻苯二甲酸酐的一种或多种,多元酸占PEN质量的510%;亚磷酸酯三苯酯占PEN质量的0.8%,酯交换和酯化反应温度为190℃~250℃;酯交换和酯化反应结束条件为:取样分析酸值为 30±5mgKOH/g,粘度为 30±10cSt,粘度计测试温度为150±5℃,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应条件为:反应釜内压力≤0.095Mpa,温度230℃~250℃;减压缩聚反应结束条件为:取样分析粘度15±10cSt,粘度计温度为200±5℃,酸值达到15±10mgKOH/g,羟值<5mgKOH/g,减压缩聚反应中反应釜内压力控制在0.09 Mpa~0.095Mpa,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,偏苯三酸酐占PEN质量的45%;十八十六叔胺占PEN质量的4.3%,聚合度调整反应条件为:反应温度 200±5℃;聚合度调整反应结束条件为:取样分析酸值为50~55mgKOH/g,粘度为25 cSt~35cSt,粘度计温度为 200±5℃,羟值<5mgKOH/g,反应结束后经过滤除去杂质即得到聚酯树脂。
Claims (9)
1.一种高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是采用回收的聚萘二甲酸乙二酯PEN废料,PEN废料粉碎后与多元醇、醇解催化剂醋酸锌或单丁基氧化锡进行醇解,醇解结束后过滤除去杂质,所得熔融体与多元酸和稳定剂亚磷酸酯三苯酯进行酯交换反应和酯化反应,酯交换反应和酯化反应结束后,进行减压缩聚反应,减压缩聚反应结束后再加入偏苯三酸酐、固化剂十八十六叔胺进行聚合度调整反应,反应结束后经过滤除去杂质即得到聚酯树脂。
2.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是多元醇为乙二醇、二甘醇、三甘醇、新戊二醇、2-甲基-1,3-丙二醇、1,3-丙二醇、丙二醇、丁二醇、特戊二醇和三羟甲基丙烷的一种或多种。
3.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是多元酸为间苯二甲酸、精对苯二甲酸、硬脂酸、己二酸、马来酸、偏苯三酸酐和邻苯二甲酸酐的一种或多种。
4.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是多元醇加入量占PEN质量的100%~300%;醋酸锌加入量占PEN质量的 0.10%~0.25%;单丁基氧化锡占PEN质量的0.25%~0.60%;多元酸占PEN质量的300%~650%;亚磷酸酯三苯酯占PEN质量的0.3%~0.8%;偏苯三酸酐占PEN质量的15%~28%;十八十六叔胺占PEN质量的2.5%~5%。
5.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是醇解温度控制在230℃~255℃。
6.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是酯交换和酯化反应温度为190℃~250℃;酯交换和酯化反应结束条件为:取样分析酸值为 30±5mgKOH/g,粘度为 30±10cSt,粘度计测试温度为150±5℃。
7.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是减压缩聚反应条件为:反应釜内压力≤0.095Mpa,温度230℃~250℃;减压缩聚反应结束条件为:取样分析粘度15±10cSt,粘度计温度为200±5℃,酸值达到15±10mgKOH/g,羟值<5mgKOH/g。
8.根据权利要求7所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是减压缩聚反应中反应釜内压力控制在0.09 Mpa~0.095Mpa。
9.根据权利要求1所述的高玻璃化温度混合型热固性粉末涂料用聚酯树脂的制备方法,其特征是聚合度调整反应条件为:反应温度 200±5℃;聚合度调整反应结束条件为:取样分析酸值为50~55mgKOH/g,粘度为25 cSt~35cSt,粘度计温度为 200±5℃,羟值<5mgKOH/g。
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