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 PDFInfo
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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
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:
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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CN104592922A (zh) * | 2014-12-31 | 2015-05-06 | 湖北绿色家园精细化工有限责任公司 | 一种透明、高硬度、耐黄变环氧饰品胶及其制备工艺 |
CN109777039A (zh) * | 2018-12-04 | 2019-05-21 | 中山大学 | 一种片式led封装用环氧树脂组合物胶饼及其制备方法和封装工艺 |
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CN104592922A (zh) * | 2014-12-31 | 2015-05-06 | 湖北绿色家园精细化工有限责任公司 | 一种透明、高硬度、耐黄变环氧饰品胶及其制备工艺 |
CN109777039A (zh) * | 2018-12-04 | 2019-05-21 | 中山大学 | 一种片式led封装用环氧树脂组合物胶饼及其制备方法和封装工艺 |
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