CN113563571A - 一种马来酸酐聚酯多元醇及其制备方法 - Google Patents
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Abstract
本发明公开了一种马来酸酐聚酯多元醇及其制备方法,它涉及漆包线漆的制备技术领域。制备方法包括以下步骤:在清洗干净的反应釜中通入氮气保护,加入乙二醇、丙二醇、丙三醇、三羟甲基丙烷、醋酸锌、正钛酸丁酯;逐步加入马来酸酐进行反应;加入己二酸进行反应脱水;保持釜温,直至反应釜精馏柱顶部温度下降,反应出液放缓;反应结束后进行取样观察,并进行送样检测粘度和酸值;利用二甲苯回流共沸将反应釜中生成的水带入分水器;在分水过程中取样检测,直至满足指标;取样检测合格后加入苯酚。本发明的优点在于:制得的马来酸酐聚酯多元醇为原料制备的聚氨酯漆包线漆,在卧式漆包机上进行涂线,涂线检测线样的性能优良,满足市场对产品的要求。
Description
技术领域
本发明涉及漆包线漆的制备技术领域,具体涉及一种马来酸酐聚酯多元醇及其制备方法。
背景技术
聚酯多元醇是聚氨酯漆包线漆重要组分之一,它是一种带有活性羟基的反应性低聚物,在涂线成膜时,聚酯多元醇中的活性羟基和游离异氰酸酯在催化剂作用下快速反应形成聚氨酯漆包线漆膜。聚氨酯漆包线漆因具有直焊性特点,满足电子、电气、电工行业等工业生产领域高速发展的要求,具有很好的应用前景。作为生产聚氨酯漆包线漆的主要原料之一的聚酯多元醇,随着聚氨酯领域的不断扩展,需求量也日益增大。目前漆包线漆行业中使用的聚酯多元醇大致有以下两种,一种是以苯酐和苯二甲酸(苯二甲酸二甲酯)为主原料的芳香族聚酯多元醇,另一种是以己二酸为主原料的饱和脂肪族聚酯多元醇。
芳香族聚酯多元醇由于分子结构中引入了苯环,虽使得聚酯多元醇具有较好的热稳定性且加工简单、价格低廉,但用来制备聚氨酯漆包线漆膜,聚氨酯漆包线漆膜的焊锡性、盐水针孔、耐热等级等性能均受到限制。从环保方面看,其结构中含有苯环,使用后较难降解,难以符合绿色环保材料的要求。脂肪族聚酯多元醇合成过程中醇酸缩聚活性虽然较高,但其强度弱,制备的聚氨酯漆包线漆的耐热等级较低,不能很好满足市场对产品的要求。
发明内容
本发明要解决的技术问题是提供一种马来酸酐聚酯多元醇及其制备方法,能够解决现有技术中芳香族聚酯多元醇制备的聚氨酯漆包线漆的焊锡性、盐水针孔、耐热等级等性能均受到限制的问题。
为解决上述技术问题,本发明的技术方案为:一种马来酸酐聚酯多元醇,由以下组分按质量份制成:
乙二醇 1-3%
丙二醇 1-3%
丙三醇 15-17%
三羟甲基丙烷 9.5-10.5%
醋酸锌 0.01-0.03%
正钛酸丁酯 0.1-0.2%
马来酸酐 18-25%
己二酸 3-10%
苯酚 35-45%
一种马来酸酐聚酯多元醇的制备方法,包括以下步骤:
S1、在清洗干净的反应釜中通入氮气保护,在搅拌状态下加入乙二醇、丙二醇、丙三醇、三羟甲基丙烷、醋酸锌、正钛酸丁酯,加料的同时升温至40-50℃,保持搅拌速度45r/min;
S2、逐步加入马来酸酐,加热升温至105-125℃进行反应2h;
S3、加入己二酸,加热升温至200-205℃进行反应脱水;
S4、保持釜温200-205℃至少3h,直至反应釜精馏柱顶部温度下降,反应出液放缓;
S5、反应结束后进行取样观察树脂是否透明,并进行送样检测粘度和酸值;
S6、维持釜温200℃,向分水器中加入二甲苯,利用二甲苯回流共沸将反应釜中生成的水带入分水器;
S7、在分水过程中每20min进行取样检测,直至满足出液称重、粘度、酸值的指标;
S8、取样检测合格后加入苯酚,进行搅拌直至树脂完全溶解,并将此树脂溶液冷却至60℃以下备用。
进一步地,所述步骤S7中,取样检测需满足以下指标:
出液称重=4.8-5.2%*投料总质量;
粘度=450-650mPa.s,以1:2 溶于间甲酚、25℃锥板测得;
酸值=0-5mg KOH/g,以溶于丁内酯测得。
本发明的优点在于:通过采用本发明设计的组分配方及生产工艺制备得到马来酸酐聚酯多元醇,将制备的马来酸酐聚酯多元醇与异氰酸酯封闭物(聚氨酯组分)、甲酚、二甲苯、正丁醛苯胺缩合物按一定比例混合均匀可制备聚氨酯漆包线漆,在卧式漆包机上进行涂线,涂线检测线样可做到拉伸3%、5%盐水零针孔,软化击穿温度可达230℃以上,同时焊锡温度330℃下可直焊,焊锡表面干净无残渣,符合耐热等级为155级新型聚氨酯漆包线漆。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施方式,对本发明进行进一步详细说明。下面的实施例可以使本专业的技术人员更全面地理解本发明,但并不因此将本发明限制在所述的实施例范围之中。
实施例1:
本具体实施方式制备一种马来酸酐聚酯多元醇,具体制备步骤如下:
S1、在清洗干净的反应釜中通入氮气保护,在搅拌状态下加入乙二醇2.5Kg、丙二醇2.8Kg、丙三醇16Kg、三羟甲基丙烷10Kg、醋酸锌20g、正钛酸丁酯120g,加料的同时升温至45℃,保持搅拌速度45r/min;
S2、逐步加入马来酸酐22Kg,加热升温至110℃进行反应2h;
S3、加入己二酸3.5Kg,加热升温至200℃进行反应脱水,期间精馏柱顶部温度为98-105℃;
S4、保持釜温200℃反应3h,精馏柱顶部温度下降至75℃,收集罐出液称重增加缓慢;
S5、反应结束后进行取样观察,并进行送样检测粘度和酸值,此时制得的马来酸酐聚酯多元醇树脂还未透明,粘度为350 mPa.s,酸值为10.8 mg KOH/g,出液称重为38.2Kg;
S6、维持釜温200℃,向分水器中加入二甲苯,利用二甲苯回流共沸将反应釜中生成的水带入分水器;
S7、将分水器中带出的水排入收集罐中,在分水过程中每20min进行取样检测,直至满足出液称重、粘度、酸值的指标;
S8、当收集罐中出液称重达到5.0Kg时,取样观察制得的马来酸酐聚酯多元醇树脂已澄清透明,粘度为515mPa.s,酸值为3.8mg KOH/g,酸值和粘度均符合要求,粘度测试仪器为Hakee VT-550锥板粘度计,测试方法为1:2溶于间甲酚/25℃锥板;
S9、加入苯酚42Kg,进行搅拌直至树脂完全溶解,并将此树脂溶液冷却至60℃以下备用。
实施例2:
本具体实施方式制备一种马来酸酐聚酯多元醇,与实施例1相比,将马来酸酐的比重降低,将己二酸的比重提高,具体制备步骤如下:
S1、在清洗干净的反应釜中通入氮气保护,在搅拌状态下加入乙二醇2.5Kg、丙二醇2.8Kg、丙三醇16Kg、三羟甲基丙烷10Kg、醋酸锌20g、正钛酸丁酯120g,加料的同时升温至45℃,保持搅拌速度45r/min;
S2、逐步加入马来酸酐18Kg,加热升温至110℃进行反应2h;
S3、加入己二酸10Kg,加热升温至200℃进行反应脱水,期间精馏柱顶部温度为98-105℃;
S4、保持釜温200℃反应3h,精馏柱顶部温度下降至75℃,收集罐出液称重增加缓慢;
S5、反应结束后进行取样观察,并进行送样检测粘度和酸值,此时制得的马来酸酐聚酯多元醇树脂还未透明,粘度为395mPa.s,酸值为12.3 mg KOH/g,出液称重为42.3Kg;
S6、维持釜温200℃,向分水器中加入二甲苯,利用二甲苯回流共沸将反应釜中生成的水带入分水器;
S7、将分水器中带出的水排入收集罐中,在分水过程中每20min进行取样检测,直至满足出液称重、粘度、酸值的指标;
S8、当收集罐中出液称重达到5.1Kg时,取样观察制得的马来酸酐聚酯多元醇树脂已澄清透明,粘度为565mPa.s,酸值为4.5mg KOH/g,酸值和粘度均符合要求,粘度测试仪器为Hakee VT-550锥板粘度计,测试方法为1:2溶于间甲酚/25℃锥板;
S9、加入苯酚42Kg,进行搅拌直至树脂完全溶解,并将此树脂溶液冷却至60℃以下备用。
将实施例1、实施例2制得的马来酸酐聚酯多元醇与异氰酸酯封闭物(聚氨酯组分)、甲酚、二甲苯、正丁醛苯胺缩合物按一定比例混合均匀制备聚氨酯漆包线漆,在卧式漆包机上进行涂线并进行检测,其测试结果见表1。
表1:实施例1和实施例2制得的马来酸酐聚酯多元醇作为原料制备的聚氨酯漆包线漆进行涂线检测的性能对比
由上表可以看出,实施例1和2制备的马来酸酐聚酯多元醇与异氰酸酯封闭物(聚氨酯组分)、甲酚、二甲苯、正丁醛苯胺缩合物按一定比例混合均匀制备聚氨酯漆包线漆,在卧式漆包机上进行涂线,涂线检测线样的焊锡性、盐水针孔、耐热等级、伸长率、耐击穿电压、热冲击性能等性能均良好。此外,实施例1、2相互比较,可看出实施例1的各项性能均优于实施例2,因而实施例1为最佳实施例。
本发明制备的马来酸酐聚酯多元醇,与其他物质按一定比例混合均匀制备的聚氨酯漆包线漆,在卧式漆包机上进行涂线,涂线检测线样的性能优良,满足市场对产品的要求。
以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (3)
2.一种权利要求1所述的马来酸酐聚酯多元醇的制备方法,其特征在于:包括以下步骤:
S1、在清洗干净的反应釜中通入氮气保护,在搅拌状态下加入乙二醇、丙二醇、丙三醇、三羟甲基丙烷、醋酸锌、正钛酸丁酯,加料的同时升温至40-50℃,保持搅拌速度45r/min;
S2、逐步加入马来酸酐,加热升温至105-125℃进行反应2h;
S3、加入己二酸,加热升温至200-205℃进行反应脱水;
S4、保持釜温200-205℃至少3h,直至反应釜精馏柱顶部温度下降,反应出液放缓;
S5、反应结束后进行取样观察树脂是否透明,并进行送样检测粘度和酸值;
S6、维持釜温200℃,向分水器中加入二甲苯,利用二甲苯回流共沸将反应釜中生成的水带入分水器;
S7、在分水过程中每20min进行取样检测,直至满足出液称重、粘度、酸值的指标;
S8、取样检测合格后加入苯酚,进行搅拌直至树脂完全溶解,并将此树脂溶液冷却至60℃以下备用。
3.根据权利要求2所述的一种马来酸酐聚酯多元醇的制备方法,其特征在于:所述步骤S7中,取样检测需满足以下指标:
出液称重=4.8-5.2%*投料总质量;
粘度=450-650mPa.s,以1:2溶于间甲酚、25℃锥板测得;
酸值=0-5mg KOH/g,以溶于丁内酯测得。
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