CN112538328A - 一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺 - Google Patents

一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺 Download PDF

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CN112538328A
CN112538328A CN202010434746.9A CN202010434746A CN112538328A CN 112538328 A CN112538328 A CN 112538328A CN 202010434746 A CN202010434746 A CN 202010434746A CN 112538328 A CN112538328 A CN 112538328A
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李俊杰
胡登华
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Wuhan Jiewei Epoxy New Material Co ltd
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Abstract

一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，其特征在于该饰品胶由A胶和B胶制成，所述A胶与B胶按1：1的质量比混合均匀后，在‑0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在110‑120℃的温度下固化1h，即得本发明。本发明提供了环氧树脂组分和固化剂组分的新配方，所得固化物外观无色透明、表面平整光滑、邵氏硬度能达到84以上、耐黄变性优良，同时操作时间长。本方法原料易得、工艺简单、成本低廉、所得固化剂性能优异，容易实现工业化。

Description

一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺
技术领域
本发明涉及一种无色透明、高硬度、耐黄变的新型环氧饰品胶的配方。尤其涉及一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺。
背景技术
传统的环氧饰品胶普遍采用聚醚胺和脂环胺体系，其中，聚醚胺包括230和403等，脂环胺包括异佛尔酮二胺IPDA、4,4，-二氨基二苯基甲烷HMDA和1,3-环己二甲胺1，3-BAC等。由于环保督查的加大，上游企业纷纷停产或减产，导致这几种做环氧饰品胶的核心原料供应不足，市场上经常出现没原料的情况，并且价格一路高涨，从而导致成本也越来越没优势，产能也严重不足，极大地限制了环氧饰品胶的健康发展，已经无法满足市场的需求。
发明内容
本发明的目的在于提供一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，以解决现有原料供应不足、价格昂贵，采购困难等技术问题，同时还可以进一步提升环氧饰品胶的性能。
为了解决上述技术问题，本发明采用的技术方案是：一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，其特征是该饰品胶由A胶和B胶制成，其工艺步骤如下：
第一步：A胶的配制：将环氧树脂128、环氧树脂E20、环氧树脂E44、聚丙二醇800、亚磷酸三苯酯、2,6-二叔丁基苯酚和抗紫外线剂UV-75投入A胶搅拌釜搅拌20-30分钟配制，其中环氧树脂128的质量份数为25～35份、环氧树脂E20的质量分数为10～20份、环氧树脂E44的质量分数为20～30份，聚丙二醇800的质量分数为15～25份、亚磷酸三苯酯的质量分数为0.1～0.3份，2,6-二叔丁基苯酚的质量分数为0.1～0.3份，抗紫外线剂UV-75的质量分数为0.3～0.5份；
第二步：B胶的合成：
（1）在反应釜中加入四氢甲基苯酐、六氢甲基苯酐、四丁基溴化铵和苄基二甲胺；其中，四氢甲基苯酐的质量份数为35～55份，六氢甲基苯酐的质量份数为20～35份，四氢基溴化铵的质量份数为0.2～0.5份，苄基二甲胺的质量份数为0.1～0.3份，1,4-丁二醇二缩水甘油醚的质量份数为5～10份，环氧树脂128的质量份数为4～8份，邻苯二甲酸二正丁酯的质量份数为20～35份，双十二碳醇酯的质量份数为0.1～0.3份；
（2）加入邻苯二甲酸二丁酯和双十二碳醇酯的混合溶液；
（3）开动搅拌，升温到60-70℃，搅拌20-30分钟；
（4）加入环氧树脂128，再升温到100-105℃，反应1-1.5h；
（5）滴加1,4-丁二醇二缩水甘油醚，滴完后保温1h，即得B胶；
第三步：环氧饰品胶制备：所述A胶与B胶按1：1的质量比混合均匀后，在-0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在110-120℃的温度下固化1h，即得本发明。
本发明提供了环氧树脂组分和固化剂组分的新配方，所得固化物外观无色透明、表面平整光滑、邵氏硬度能达到84以上、耐黄变性优良，同时操作时间长。本方法原料易得、工艺简单、成本低廉、所得固化剂性能优异，容易实现工业化。
具体实施方式
下面结合具体实施例，对本发明的实施方法做进一步详细说明。
实施例1
一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，该饰品胶由A胶和B胶制成，其工艺步骤如下：
A胶的配制：
将25份（质量份数，下同）环氧树脂128、10份环氧树脂E20、30份环氧树脂E44、25份聚丙二醇800、0.1份亚磷酸三苯酯、0.3份2,6-二叔丁基苯酚和0.5份抗紫外线剂UV-75投入A胶搅拌釜搅拌30分钟，即得A胶。
B胶的合成：
（1）在反应釜中加入35份四氢甲基苯酐、35份六氢甲基苯酐、0.2份四丁基溴化铵和0.3份苄基二甲胺；
（2）加入20份邻苯二甲酸二丁酯和0.1份双十二碳醇酯的混合溶液；
（3）开动搅拌，升温到60℃，搅拌20分钟；
（4）加入4份环氧树脂128，再升温到102℃，反应1.5h；
（5）滴加10份1,4-丁二醇二缩水甘油醚，滴完后保温1h，即得B胶。
环氧饰品胶制备：
所述A胶与B胶按1：1的质量比混合均匀后，在-0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在115℃的温度下固化1h，所得固化物无色透明、表面平整光滑、邵氏硬度能达到84以上、耐黄变性优良，同时操作时间达到24h，操作方便。
实施例2
一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，该饰品胶由A胶和B胶制成，其工艺步骤如下：
A胶的配制：
将35份（质量份数，下同）环氧树脂128、15份环氧树脂E20、25份环氧树脂E44、25份聚丙二醇800、0.3份亚磷酸三苯酯、0.1份2,6-二叔丁基苯酚和0.3份抗紫外线剂UV-75投入A胶搅拌釜搅拌25分钟，即得A胶。
B胶的合成：
（1）在反应釜中加入55份四氢甲基苯酐、20份六氢甲基苯酐、0.5份四丁基溴化铵和0.1份苄基二甲胺；
（2）然后加入20份邻苯二甲酸二丁酯和0.3份双十二碳醇酯的混合溶液
（3）开动搅拌，升温到65℃，搅拌20分钟；
（4）加入8份环氧树脂128，再升温到105℃，反应1h；
（5）滴加5份1,4-丁二醇二缩水甘油醚，滴完后保温1h，即得B胶。
环氧饰品胶制备：所述A胶与B胶按1：1的质量比混合均匀后，在-0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在120℃的温度下固化1h，所得固化物无色透明、表面平整光滑、邵氏硬度能达到86以上、耐黄变性优良，同时操作时间达到24h，操作方便。
实施例3
一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，该饰品胶由A胶和B胶制成，其工艺步骤如下：
A胶的配制：
将30份（质量份数，下同）环氧树脂128、20份环氧树脂E20、30份环氧树脂E44、20份聚丙二醇800、0.2份亚磷酸三苯酯、0.2份2,6-二叔丁基苯酚和0.4份抗紫外线剂UV-75投入A胶搅拌釜搅拌20分钟，即得A胶。
B胶的合成：
（1）在反应釜中加入45份四氢甲基苯酐、28份六氢甲基苯酐、0.35份四丁基溴化铵和0.2份苄基二甲胺；
（2）加入20份邻苯二甲酸二丁酯和0.2份双十二碳醇酯的混合溶液；
（3）开动搅拌，升温到70℃，搅拌20分钟；
（4）加入6份环氧树脂128，再升温到100℃，反应1.2h；
（5）滴加8份1,4-丁二醇二缩水甘油醚，滴完后保温1h，即得B胶。
环氧饰品胶制备：所述A胶与B胶按1：1的质量比混合均匀后，在-0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在110℃的温度下固化1h，所得固化物无色透明、表面平整光滑、邵氏硬度能达到85以上、耐黄变性优良，同时操作时间达到24h，操作方便。
为了进一步验证以上实施例的效果，将本发明与其他公司产品进行性能对比试验，试验数据如下表所示：
Figure 395855DEST_PATH_IMAGE002

Claims (1)

1.一种无色透明、高硬度、耐黄变的新型环氧饰品胶的制备工艺，其特征在于该饰品胶由A胶和B胶制成，其工艺步骤如下：
第一步：A胶的配制：
将环氧树脂128、环氧树脂E20、环氧树脂E44、聚丙二醇800、亚磷酸三苯酯、2,6-二叔丁基苯酚和抗紫外线剂UV-75投入A胶搅拌釜搅拌20-30分钟配制，其中环氧树脂128的质量份数为25～35份、环氧树脂E20的质量分数为10～20份、环氧树脂E44的质量分数为20～30份，聚丙二醇800的质量分数为15～25份、亚磷酸三苯酯的质量分数为0.1～0.3份，2,6-二叔丁基苯酚的质量分数为0.1～0.3份，抗紫外线剂UV-75的质量分数为0.3～0.5份；
第二步：B胶的合成：
在反应釜中加入四氢甲基苯酐、六氢甲基苯酐、四丁基溴化铵和苄基二甲胺；其中，四氢甲基苯酐的质量份数为35～55份，六氢甲基苯酐的质量份数为20～35份，四氢基溴化铵的质量份数为0.2～0.5份，苄基二甲胺的质量份数为0.1～0.3份，1,4-丁二醇二缩水甘油醚的质量份数为5～10份，环氧树脂128的质量份数为4～8份，邻苯二甲酸二正丁酯的质量份数为20～35份，双十二碳醇酯的质量份数为0.1～0.3份；
加入邻苯二甲酸二丁酯和双十二碳醇酯的混合溶液；
开动搅拌，升温到60-70℃，搅拌20-30分钟；
加入环氧树脂128，再升温到100-105℃，反应1-1.5h；
滴加1,4-丁二醇二缩水甘油醚，滴完后保温1h，即得B胶；
第三步：环氧饰品胶制备：
所述A胶与B胶按1：1的质量比混合均匀后，在-0.1MPa的真空箱中消泡，然后分装到硅胶模具中，在110-120℃的温度下固化1h，即得本发明。
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