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

Info

Publication number
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
Authority
CN
China
Prior art keywords
mass fraction
parts
adhesive
epoxy resin
glue
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010434746.9A
Other languages
English (en)
Inventor
李俊杰
胡登华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Jiewei Epoxy New Material Co ltd
Original Assignee
Wuhan Jiewei Epoxy New Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Jiewei Epoxy New Material Co ltd filed Critical Wuhan Jiewei Epoxy New Material Co ltd
Priority to CN202010434746.9A priority Critical patent/CN112538328A/zh
Publication of CN112538328A publication Critical patent/CN112538328A/zh
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
    • C08G59/4284—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof together with other curing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5033—Amines aromatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/56—Amines together with other curing agents
    • C08G59/58—Amines together with other curing agents with polycarboxylic acids or with anhydrides, halides, or low-molecular-weight esters thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/10—Transparent films; Clear coatings; Transparent materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Epoxy Resins (AREA)

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。
CN202010434746.9A 2020-05-21 2020-05-21 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 Pending CN112538328A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010434746.9A CN112538328A (zh) 2020-05-21 2020-05-21 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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010434746.9A CN112538328A (zh) 2020-05-21 2020-05-21 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

Publications (1)

Publication Number Publication Date
CN112538328A true CN112538328A (zh) 2021-03-23

Family

ID=75013361

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010434746.9A Pending CN112538328A (zh) 2020-05-21 2020-05-21 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

Country Status (1)

Country Link
CN (1) CN112538328A (zh)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Similar Documents

Publication Publication Date Title
CN107805207A (zh) 一种聚天门冬氨酸酯的制备方法
CN104403089A (zh) 一种改性环氧脂环胺高性能固化剂及其制备方法
CN112125927A (zh) 一种含有弹性体的硅烷偶联剂及其制备方法
CN103449979A (zh) 一种双酚环氧树脂及其制备方法
CN107501859A (zh) 一种用于环氧树脂体系的dopo型固化剂及其应用
CN112538328A (zh) 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
CN114479739B (zh) 一种环氧树脂胶及其在一次性制作透明制品中的应用
CN103013419B (zh) 银行卡复合用粘合剂及其制备方法
CN102337013B (zh) 改性环氧树脂板
CN102850497B (zh) 一种脲醛树脂胶粘剂的制备方法
CN112358602A (zh) 一种环氧磷酸酯树脂及其制备方法
CN114213629A (zh) 固化剂、固化剂组合物及其制备方法
CN114369405A (zh) 环氧美缝剂及其制备方法
CN109233710B (zh) 一种具有高玻璃化转变温度、高温粘结性的绝缘材料及其制备方法
CN113912960A (zh) 一种透明pvc复合薄膜及其制备方法
CN106380576A (zh) 一种新型曼尼期碱环氧树脂固化剂
CN111634102A (zh) 一种epe珍珠棉和铝膜复合工艺
CN105199068A (zh) 聚氨酯丙烯酸酯合成工艺
CN113461960B (zh) 一种超支化水性环氧树脂固化剂的制备方法
CN114524784A (zh) 一种耐黄变、高防腐的腰果酚环氧固化剂制备方法
CN110903798A (zh) 一种木材金属复合胶粘剂
CN114163956B (zh) 一种胶水的制备工艺及应用
CN113243610B (zh) 一种鞋底耐酸碱的安全鞋及其制备方法
CN109265323A (zh) 一种窄分子量分布双酚a聚氧乙烯醚的制备方法
CN109897568B (zh) 一种美缝剂用耐白化固化剂及其制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination