CN104059590B - A kind of self-vulcanizing toughened epoxy resin adhesive and preparation method thereof - Google Patents
A kind of self-vulcanizing toughened epoxy resin adhesive and preparation method thereof Download PDFInfo
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Abstract
本发明涉及一种室温固化增韧环氧树脂胶粘剂及其制备方法，属于高分子材料技术领域。本发明的环氧树脂胶粘剂包括以下按照重量份数计的原料：环氧树脂40-60份、固化剂30-50份、环氧化聚丁二烯10-20份、对苯二甲酸二辛酯10-18份、硅烷偶联剂3-5份、碳酸钙30-50份。本发明制备的环氧树脂胶粘剂，既能室温固化，又具有较佳的韧性，具有较为广泛的应用。本专利通过在室温固化环氧树脂中添加增韧剂的技术途径对环氧树脂进行增韧改性，以使其能较好地应用于各种制备工艺不同、应用目的不同的室温固化环氧树脂胶粘剂的制备，能够很好地应用于芳纶纤维复合材料。The invention relates to a room temperature curing and toughening epoxy resin adhesive and a preparation method thereof, belonging to the technical field of polymer materials. The epoxy resin adhesive of the present invention comprises the following raw materials in parts by weight: 40-60 parts of epoxy resin, 30-50 parts of curing agent, 10-20 parts of epoxidized polybutadiene, dioctyl terephthalate 10-18 parts of ester, 3-5 parts of silane coupling agent, 30-50 parts of calcium carbonate. The epoxy resin adhesive prepared by the invention can not only be cured at room temperature, but also has better toughness, and has wider application. This patent toughens and modifies the epoxy resin through the technical approach of adding a toughening agent to the room temperature curing epoxy resin, so that it can be better applied to various room temperature curing epoxy resins with different preparation processes and different application purposes. The preparation of the resin adhesive can be well applied to the aramid fiber composite material.
Description
技术领域 technical field
本发明涉及一种环氧树脂胶粘剂及其制备方法，更具体地说，本发明涉及一种室温固化增韧环氧树脂胶粘剂及其制备方法，属于高分子材料技术领域。 The invention relates to an epoxy resin adhesive and a preparation method thereof. More specifically, the invention relates to a room temperature curing toughened epoxy resin adhesive and a preparation method thereof, belonging to the technical field of polymer materials.
背景技术 Background technique
环氧树脂是一种热固性树脂，因具有优异的粘接性、机械强度及电绝缘性等特性，而广泛应用于胶粘剂、高性能-轻重量纤维增强复合材料、涂料和复合材料基体等方面。此外，环氧树脂胶粘剂由于其良好的性能被广泛用于结构胶粘剂。但其明显的脆性以及较差的耐气候性、耐疲劳性、耐热性、吸湿性和抗冲击性能使其在高应力下承受外加作用力的能力较差，是它无法避免的缺点。因此，需要对环氧树脂进行改性。此外，由于环氧树脂粘度较高、对芳纶纤维的浸润性差等特点，要将环氧树脂很好地用于芳纶纤维复合材料的制备，必须对环氧树脂进行必要的改性，使所制备的芳纶/环氧树脂复合材料具有最佳的综合性能。 Epoxy resin is a kind of thermosetting resin, which is widely used in adhesives, high-performance-light-weight fiber-reinforced composite materials, coatings and composite material substrates due to its excellent adhesion, mechanical strength and electrical insulation properties. In addition, epoxy resin adhesives are widely used in structural adhesives due to their good properties. However, its obvious brittleness and poor weather resistance, fatigue resistance, heat resistance, moisture absorption and impact resistance make it less able to withstand external forces under high stress, which is an unavoidable shortcoming. Therefore, it is necessary to modify the epoxy resin. In addition, due to the high viscosity of epoxy resin and poor wettability to aramid fiber, epoxy resin must be modified to make aramid fiber composite material well. The prepared aramid fiber/epoxy resin composite has the best comprehensive properties.
国家知识产权局于2008.4.9公开了一件公开号为CN101157835，名称为“一种改性环氧树脂胶粘剂及其应用”的发明专利，该专利提供一种能够有效固定弹簧、使得弹簧不容易从弹簧槽脱落的胶粘剂。本发明同时提供这种胶粘剂在固定弹簧方面的应用。本发明的改性环氧树脂胶粘剂，包括以下质量份的组分：环氧树脂100；聚硫胶50~200；白炭黑5~15；偶联剂1~5；胺类固化剂2~10。与普通环氧树脂相比：本发明采用聚硫橡胶对环氧树脂进行改性，它是一种反应性液态聚合增韧的方法，当聚硫橡胶与环氧树脂混合后，聚硫胶中的硫醇基与环氧基发生反应，参加到固化的环氧树脂结构中，赋予环氧树脂良好的柔韧性。因此本发明的改性环氧树脂胶粘剂能有效固定弹簧、使得弹簧不容易从弹簧槽脱落，同时又保持了环氧树脂的其他有效性能。 The State Intellectual Property Office published an invention patent with the publication number CN101157835 titled "A Modified Epoxy Resin Adhesive and Its Application" on April 9, 2008. This patent provides a method that can effectively fix the spring so that the spring is not easy Adhesive that has come off the spring groove. The invention also provides the application of the adhesive in fixing springs. The modified epoxy resin adhesive of the present invention comprises the following components by mass: epoxy resin 100; polysulfide glue 50~200; white carbon black 5~15; coupling agent 1~5; amine curing agent 2~ 10. Compared with ordinary epoxy resin: the present invention uses polysulfide rubber to modify epoxy resin, which is a method of reactive liquid polymerization toughening. When polysulfide rubber is mixed with epoxy resin, the polysulfide rubber The thiol group reacts with the epoxy group and participates in the cured epoxy resin structure, endowing the epoxy resin with good flexibility. Therefore, the modified epoxy resin adhesive of the present invention can effectively fix the spring so that the spring is not easy to fall off from the spring groove, while maintaining other effective properties of the epoxy resin.
上述专利中的环氧树脂胶粘剂有一定柔韧性，但是综合性能不佳，无法很好地应用于芳纶纤维复合材料。 The epoxy resin adhesive in the above-mentioned patent has certain flexibility, but its overall performance is not good, so it cannot be well applied to aramid fiber composite materials.
发明内容 Contents of the invention
本发明旨在解决上述技术问题，提供一种室温固化增韧环氧树脂胶粘剂，提高其综合性能，使其能够很好地应用于芳纶纤维复合材料。 The present invention aims to solve the above-mentioned technical problems, provide a room-temperature-cured and toughened epoxy resin adhesive, improve its comprehensive performance, and enable it to be well applied to aramid fiber composite materials.
为了实现上述发明目的，其具体的技术方案如下： In order to realize the above-mentioned purpose of the invention, its concrete technical scheme is as follows:
一种室温固化增韧环氧树脂胶粘剂，其特征在于：包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive is characterized in that: comprising the following raw materials in parts by weight:
环氧树脂 40-60份 Epoxy resin 40-60 parts
固化剂 30-50份 Curing agent 30-50 parts
环氧化聚丁二烯 10-20份 Epoxidized polybutadiene 10-20 parts
对苯二甲酸二辛酯 10-18份 Dioctyl terephthalate 10-18 parts
硅烷偶联剂 3-5份 Silane coupling agent 3-5 parts
碳酸钙 30-50份。 Calcium carbonate 30-50 parts.
一种室温固化增韧环氧树脂胶粘剂，其特征在于：包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive is characterized in that: comprising the following raw materials in parts by weight:
环氧树脂 45-55份 Epoxy resin 45-55 parts
固化剂 35-43份 Curing agent 35-43 parts
环氧化聚丁二烯 12-17份 Epoxidized polybutadiene 12-17 parts
对苯二甲酸二辛酯 11-15份 Dioctyl terephthalate 11-15 parts
硅烷偶联剂 4-4.5份 Silane coupling agent 4-4.5 parts
碳酸钙 35-40份。 Calcium carbonate 35-40 parts.
本发明所述的环氧树脂为E-44环氧树脂。 The epoxy resin described in the present invention is E-44 epoxy resin.
本发明所述的固化剂为554固化剂。 The curing agent described in the present invention is 554 curing agent.
本发明所述的硅烷偶联剂为KH-550硅烷偶联剂。 The silane coupling agent described in the present invention is KH-550 silane coupling agent.
一种室温固化增韧环氧树脂胶粘剂的制备方法，其特征在于：包括以下工艺步骤： A preparation method of room temperature curing toughened epoxy resin adhesive, characterized in that: comprising the following process steps:
A、按配方要求称取环氧树脂、环氧化聚丁二烯、硅烷偶联剂及碳酸钙，搅拌混合； A. Take epoxy resin, epoxidized polybutadiene, silane coupling agent and calcium carbonate according to the formula requirements, stir and mix;
B、于双辊或三辊机上进一步混合均匀为A组分，备用； B. Further mix evenly on a two-roller or three-roller machine to form A component, and set aside;
C、按配方要求称取固化剂和对苯二甲酸二辛酯，混合后得到B组分，备用； C. Weigh the curing agent and dioctyl terephthalate according to the formula requirements, mix to obtain component B, and set aside;
D、取步骤B得到的A组分和步骤C得到的B组分，混合，于室温下固化，得到环氧树脂胶粘剂。 D. Take component A obtained in step B and component B obtained in step C, mix and cure at room temperature to obtain an epoxy resin adhesive.
本发明带来的有益技术效果： Beneficial technical effects brought by the present invention:
本发明解决了现有环氧树脂胶粘剂综合性能不佳，无法很好地应用于芳纶纤维复合材料的问题，本发明制备的环氧树脂胶粘剂，既能室温固化，又具有较佳的韧性，具有较为广泛的应用。本专利通过在室温固化环氧树脂中添加增韧剂的技术途径对环氧树脂进行增韧改性，以使其能较好地应用于各种制备工艺不同、应用目的不同的室温固化环氧树脂胶粘剂的制备，能够很好地应用于芳纶纤维复合材料。 The invention solves the problem that the existing epoxy resin adhesive has poor comprehensive performance and cannot be well applied to aramid fiber composite materials. The epoxy resin adhesive prepared by the invention can be cured at room temperature and has better toughness. Has a wider range of applications. This patent toughens and modifies the epoxy resin through the technical approach of adding a toughening agent to the room temperature curing epoxy resin, so that it can be better applied to various room temperature curing epoxy resins with different preparation processes and different application purposes. The preparation of the resin adhesive can be well applied to the aramid fiber composite material.
具体实施方式 Detailed ways
实施例1Example 1
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 40份 Epoxy resin 40 parts
固化剂 30份 Curing agent 30 parts
环氧化聚丁二烯 10份 Epoxidized polybutadiene 10 parts
对苯二甲酸二辛酯 10份 Dioctyl terephthalate 10 parts
硅烷偶联剂 3份 Silane coupling agent 3 parts
碳酸钙 30份。 Calcium Carbonate 30 parts.
实施例2Example 2
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 60份 Epoxy resin 60 parts
固化剂 50份 Curing agent 50 parts
环氧化聚丁二烯 20份 Epoxidized polybutadiene 20 parts
对苯二甲酸二辛酯 18份 Dioctyl terephthalate 18 parts
硅烷偶联剂 5份 Silane coupling agent 5 parts
碳酸钙 50份。 Calcium Carbonate 50 parts.
实施例3Example 3
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 50份 Epoxy resin 50 parts
固化剂 40份 Curing agent 40 parts
环氧化聚丁二烯 15份 Epoxidized polybutadiene 15 parts
对苯二甲酸二辛酯 14份 Dioctyl terephthalate 14 parts
硅烷偶联剂 4份 Silane coupling agent 4 parts
碳酸钙 40份。 Calcium Carbonate 40 parts.
实施例4Example 4
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 46份 Epoxy resin 46 parts
固化剂 33份 Curing agent 33 parts
环氧化聚丁二烯 19份 Epoxidized polybutadiene 19 parts
对苯二甲酸二辛酯 15份 Dioctyl terephthalate 15 parts
硅烷偶联剂 3.5份 Silane coupling agent 3.5 parts
碳酸钙 48份。 Calcium Carbonate 48 parts.
实施例5Example 5
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 45份 Epoxy resin 45 parts
固化剂 35份 Curing agent 35 parts
环氧化聚丁二烯 12份 Epoxidized polybutadiene 12 parts
对苯二甲酸二辛酯 11份 Dioctyl terephthalate 11 parts
硅烷偶联剂 4份 Silane coupling agent 4 parts
碳酸钙 35份。 Calcium carbonate 35 parts.
实施例6Example 6
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 55份 Epoxy resin 55 parts
固化剂 43份 Curing agent 43 parts
环氧化聚丁二烯 17份 Epoxidized polybutadiene 17 parts
对苯二甲酸二辛酯 15份 Dioctyl terephthalate 15 parts
硅烷偶联剂 4.5份 Silane coupling agent 4.5 parts
碳酸钙 40份。 Calcium Carbonate 40 parts.
实施例7Example 7
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 50份 Epoxy resin 50 parts
固化剂 39份 Curing agent 39 parts
环氧化聚丁二烯 14.5份 Epoxidized polybutadiene 14.5 parts
对苯二甲酸二辛酯 13份 Dioctyl terephthalate 13 parts
硅烷偶联剂 4.25份 Silane coupling agent 4.25 parts
碳酸钙 37.5份。 Calcium carbonate 37.5 parts.
实施例8Example 8
一种室温固化增韧环氧树脂胶粘剂，包括以下按照重量份数计的原料： A room temperature curing toughened epoxy resin adhesive, comprising the following raw materials in parts by weight:
环氧树脂 47份 Epoxy resin 47 parts
固化剂 36份 Curing agent 36 parts
环氧化聚丁二烯 16.5份 Epoxidized polybutadiene 16.5 parts
对苯二甲酸二辛酯 14.5份 Dioctyl terephthalate 14.5 parts
硅烷偶联剂 4.2份 Silane coupling agent 4.2 parts
碳酸钙 38份。 Calcium Carbonate 38 parts.
实施例9Example 9
在实施例1-9的基础上，优选的： On the basis of embodiment 1-9, preferably:
所述的环氧树脂为E-44环氧树脂。 Described epoxy resin is E-44 epoxy resin.
所述的固化剂为554固化剂。 Described curing agent is 554 curing agents.
所述的硅烷偶联剂为KH-550硅烷偶联剂。 The silane coupling agent is KH-550 silane coupling agent.
实施例10Example 10
一种室温固化增韧环氧树脂胶粘剂的制备方法，包括以下工艺步骤： A preparation method of room temperature curing toughened epoxy resin adhesive, comprising the following process steps:
A、按配方要求称取环氧树脂、环氧化聚丁二烯、硅烷偶联剂及碳酸钙，搅拌混合； A. Take epoxy resin, epoxidized polybutadiene, silane coupling agent and calcium carbonate according to the formula requirements, stir and mix;
B、于双辊或三辊机上进一步混合均匀为A组分，备用； B. Further mix evenly on a two-roller or three-roller machine to form A component, and set aside;
C、按配方要求称取固化剂和对苯二甲酸二辛酯，混合后得到B组分，备用； C. Weigh the curing agent and dioctyl terephthalate according to the formula requirements, mix to obtain component B, and set aside;
D、取步骤B得到的A组分和步骤C得到的B组分，混合，于室温下固化，得到环氧树脂胶粘剂。 D. Take component A obtained in step B and component B obtained in step C, mix and cure at room temperature to obtain an epoxy resin adhesive.
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