CN105949445B - 一种聚氨酯固化剂用中间体及固化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种聚氨酯固化剂用中间体,组成组分按质量百分比为:21%‑26.74%苯酐、5.93%‑9.21%苯甲酸、0%‑20.19%十二酸、0%‑25.84%十六酸、0%‑10.01%季戊四醇、0.16%‑0.18%次磷酸、20.19%‑26.00%甘油、8.01%‑25.83%二甲苯、0%‑19.69%乙酸乙酯,同时还公开了其制作方法以及由其制成的聚氨酯固化剂。本发明的聚氨酯固化剂用中间体以醇类甘油或季戊四醇来替代比较活泼的TMP,使得反应平缓,易控制,用一元酸的十二酸或十六酸替代部分苯酐,在合成过程中可以有效的控制反应速度,降低游离TDI的含量,提高中间体的相溶性及光泽。
Description
技术领域
本发明涉及聚氨酯材料领域,特别涉及一种聚氨酯固化剂用中间体及其制备方法,同时还涉及由该固化剂用中间体制成的固化剂及其制备方法。
背景技术
聚氨酯涂料性能优异,自诞生以来,迅速成为最为重要和应用最广泛的涂料品种。广泛应用于各个涂料领域,聚氨酯涂料被广泛作为汽车涂料,木器涂料,建筑外墙涂料,金属防腐涂料。
聚氨酯涂料的漆膜具有硬度高,柔韧性好,耐磨和耐化学品的能力强,干燥快等优点,因此聚氨酯在国内的发展很迅速,是溶剂型涂料的重要品种之一。聚氨酯涂料在家居与装修中用量一直比较大,在家居涂料中占据着统治地位。
甲苯二异氰酸酯单体(TDI)的官能度低,在醋酸乙酯,醋酸丁酯等酯类溶剂中醇酸稳定性不佳,与羟基丙烯酸树脂和醇酸树脂的相溶性不好,不适合直接作为涂料固化剂。目前,国内最常用的聚氨酯固化剂的生产方法是采用三羟甲基丙烷(TMP)与甲苯二异氰酸酯(TDI)反应加成,称为TDI-TMP加成物或预聚体。反应原理是利用TDI苯环上的4号位-NCO基团比2号位的-NCO基团更活跃,反应快的特点,使其预留苯环上2号位上的-NCO基,形成含有一定游离NCO基团的TDI-TMP加成物固化剂。
但是,TDI-TMP体系聚氨酯固化剂用于配制面漆漆膜易发脆,且随着树脂品种的多样化,普遍存在相溶性差,光泽不好的问题。
发明内容
本发明要解决的技术问题是提供一种聚氨酯固化剂用中间体,用于涂料中可明显改善相容性差的问题,提高涂料的柔韧性、容忍度和光泽,同时该聚氨酯固化剂用中间体原材料丰富,生产成本低廉。
为了解决上述技术问题,本发明的技术方案为,一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
一种聚氨酯固化剂用中间体的制备方法:
步骤1,通氮气,先将液体料甘油﹑次磷酸和回流二甲苯依次投入反应釜中,然后依次投入固体料十二酸﹑十六酸﹑苯甲酸﹑苯酐﹑季戊四醇;
步骤2,开始缓慢升温,并开回流冷却水,待大部分物料融化的时候,开始搅拌,搅拌开始后继续升温,待回流稳定后,停止通氮气;
步骤3,将反应温度缓慢升至190℃,并在190℃~215℃反应温度下,回流酯化2h后取样滴定固体酸值,当固体酸值2.0-3.0mgKOH/g时,通氮气,冷却至150℃以下,加入兑稀溶剂二甲苯和乙酸乙酯进行兑稀,搅拌均匀后取样调粘至要求的指标,即得到聚氨酯固化剂用中间体。
一种由聚氨酯固化剂用中间体制成的聚氨酯固化剂,其组成组分按质量百分比如下:
聚氨酯固化剂用中间体:45.78%
甲苯二异氰酸酯TDI:18.39%
二甲苯:21.05%
醋酸丁酯:7.39%
醋酸乙酯:7.39%;
制备方法为:先将甲苯二异氰酸酯TDI投入反应釜中,开搅拌,然后依次投入聚氨酯固化剂用中间体、二甲苯、醋酸乙酯、醋酸丁酯,缓慢升温至98℃,在98-105℃之间保温2小时,测粘度,NCO含量,固体份,达到指标后,搅拌均匀,即可得到成品。
采用上述技术方案,以醇类甘油或季戊四醇来替代传统生产方式用的比较活泼的TMP,使得反应较为平缓,易控制,同时用一元酸的十二酸或十六酸替代部分苯酐,使得在间体合成聚氨酯固化剂的过程中,可以有效的控制反应速度,降低游离TDI的含量,提高中间体的相溶性及光泽。
具体实施方式
下面对本发明的具体实施方式作进一步说明。在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
本实施例聚氨酯固化剂用中间体的制备方法:
步骤1,通氮气,先将液体料甘油﹑次磷酸和回流二甲苯依次投入反应釜中,然后依次投入固体料十二酸﹑苯甲酸﹑苯酐﹑季戊四醇;
步骤2,开始缓慢升温,并开回流冷却水,待大部分物料融化的时候,开始搅拌,搅拌开始后继续升温,待回流稳定后,停止通氮气;
步骤3,将反应温度缓慢升至190℃,并在190℃~215℃反应温度下,回流酯化2h后取样滴定固体酸值,当固体酸值2.0-3.0mgKOH/g时,通氮气,冷却至150℃以下,加入兑稀溶剂二甲苯和乙酸乙酯进行兑稀,搅拌均匀后取样调粘至要求的指标,即得到聚氨酯固化剂用中间体。
实施例2
一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
制备方法与实施例1相同。
实施例3
一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
制备方法与实施例1相同。
实施例4
一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
制备方法与实施例1相同。
实施例5
一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
制备方法与实施例1相同。
聚氨酯固化剂用中间体的性能如下表所示:
酸值采用传统的氢氧化钾滴定法,而色泽采用铁-钴(Fe-Co)比色法
以实施例1~5所得的聚氨酯固化剂用中间体制备聚氨酯固化剂,其组成组分按质量百分比如下:
聚氨酯固化剂用中间体:45.78%
甲苯二异氰酸酯TDI:18.39%
二甲苯:21.05%
醋酸丁酯:7.39%
醋酸乙酯:7.39%;
制备方法为:先将甲苯二异氰酸酯TDI投入反应釜中,开搅拌,然后依次投入聚氨酯固化剂用中间体、二甲苯、醋酸乙酯、醋酸丁酯,缓慢升温至98℃,在98-105℃之间保温2小时,测粘度,NCO含量,固体份,达到指标后,搅拌均匀,即可得到成品。
所得的聚氨酯固化剂依次定义为实施例6~10
所制得的聚氨酯固化剂的性能如下:
其中,NCO%值是指100g试样所含的异氰酸酯(-NCO)基团的质量百分比,而粘度采用涂4粘度杯进行测试。
以上对本发明的实施方式作了详细说明,但本发明不限于所描述的实施方式。对于本领域的技术人员而言,在不脱离本发明原理和精神的情况下,对这些实施方式进行多种变化、修改、替换和变型,仍落入本发明的保护范围内。
Claims (2)
1.一种聚氨酯固化剂用中间体,其组成组分按质量百分比如下:
制备所述的聚氨酯固化剂用中间体的方法,制备步骤如下:
步骤1,通氮气,先将液体料甘油﹑次磷酸和回流二甲苯依次投入反应釜中,然后依次投入固体料十二酸﹑十六酸﹑苯甲酸﹑苯酐﹑季戊四醇;
步骤2,开始缓慢升温,并开回流冷却水,待大部分物料融化的时候,开始搅拌,搅拌开始后继续升温,待回流稳定后,停止通氮气;
步骤3,将反应温度缓慢升至190℃,并在190℃~215℃反应温度下,回流酯化2h后取样滴定固体酸值,当固体酸值2.0-3.0mgKOH/g时,通氮气,冷却至150℃以下,加入兑稀溶剂二甲苯和乙酸乙酯进行兑稀,搅拌均匀后取样调粘至要求的指标,即得到聚氨酯固化剂用中间体。
2.一种由权利要求1所述的聚氨酯固化剂用中间体制成的聚氨酯固化剂,其特征在于,其组成组分按质量百分比如下:
制备方法为:先将甲苯二异氰酸酯TDI投入反应釜中,开搅拌,然后依次投入聚氨酯固化剂用中间体、二甲苯、醋酸乙酯、醋酸丁酯,缓慢升温至98℃,在98-105℃之间保温2小时,测粘度,NCO含量,固体份,达到指标后,搅拌均匀,即可得到成品。
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