阅读说明：本技术 一种具有高韧性且无毒的环氧树脂胶配方及其制备方法 (Formula and preparation method of high-toughness and non-toxic epoxy resin adhesive ) 是由 李卫东 于 2021-08-02 设计创作，主要内容包括：本发明公开了一种具有高韧性且无毒的环氧树脂胶配方及其制备方法,以重量份计算,包括如下原料组分：E-44环氧树脂80-100份；β-环糊精复合物10-20份；玻璃纤维粉8-15份；滑石粉5-10份；混合溶剂20-40份；消泡剂0.2-5份；固化剂2-5份；制备方法为先将E-44环氧树脂、β-环糊精复合物、玻璃纤维粉和滑石粉加入到反应釜中,并且加热至50-70℃,搅拌1-1.5小时；再将混合溶剂和固化剂加入到上述混合物中,并且加热至50-70℃,搅拌0.5-1小时；最后把消泡剂加入到上述混合物中,并且加热至40-50℃,搅拌0.5-1小时,之后冷却2-3小时至室温,出料。本发明固化后涂抹性极好,粘结性能极好,其分子内既具有耐热性好的硬段,又具有柔韧性好的软段,胶黏剂脆性小,增韧作用明显。(The invention discloses a high-toughness and non-toxic epoxy resin adhesive formula and a preparation method thereof, wherein the epoxy resin adhesive comprises the following raw material components in parts by weight: 80-100 parts of E-44 epoxy resin; 10-20 parts of beta-cyclodextrin compound; 8-15 parts of glass fiber powder; 5-10 parts of talcum powder; 20-40 parts of a mixed solvent; 0.2-5 parts of a defoaming agent; 2-5 parts of a curing agent; the preparation method comprises the steps of firstly adding the E-44 epoxy resin, the beta-cyclodextrin compound, the glass fiber powder and the talcum powder into a reaction kettle, heating to 50-70 ℃, and stirring for 1-1.5 hours; adding the mixed solvent and the curing agent into the mixture, heating to 50-70 ℃, and stirring for 0.5-1 hour; and finally, adding the defoaming agent into the mixture, heating to 40-50 ℃, stirring for 0.5-1 hour, cooling for 2-3 hours to room temperature, and discharging. The invention has excellent smearing property after curing and bonding property, has a hard segment with good heat resistance and a soft segment with good flexibility in a molecule, and has small brittleness and obvious toughening effect.)

1. The formula of the high-toughness and non-toxic epoxy resin adhesive is characterized by comprising the following raw material components in parts by weight:

2. the formulation of claim 1, wherein the solvent mixture is prepared by mixing ethanol and n-butanol at a mass ratio of 8: 2.

3. The formulation of claim 1, wherein the beta-cyclodextrin complex is prepared by the following steps: stirring beta-cyclodextrin, sodium hydroxide and pyridine, adding succinic anhydride, heating, stirring, adding dimethylformamide for crystallization, drying, adding sodium montmorillonite and water, stirring, adding tetradecyl tributyl ammonium chloride and dodecyl tributyl ammonium bromide, heating, stirring, filtering, washing solid with anhydrous ethanol, drying in air atmosphere, and pulverizing to obtain beta-cyclodextrin complex.

4. A preparation method of a nontoxic epoxy resin adhesive with high toughness is characterized by comprising the following steps:

the first step is as follows: adding E-44 epoxy resin, beta-cyclodextrin compound, glass fiber powder and talcum powder into a reaction kettle, heating to 50-70 ℃, and stirring for 1-1.5 hours;

the second step is that: adding the mixed solvent and the curing agent into the mixture in the first step, heating to 50-70 ℃, and stirring for 0.5-1 hour;

the third step: adding defoaming agent into the mixture of the second step, heating to 40-50 deg.c, stirring for 0.5-1 hr, cooling for 2-3 hr to room temperature and discharging.

Technical Field

The invention relates to the technical field of epoxy resin, in particular to a formula of a high-toughness and non-toxic epoxy resin adhesive and a preparation method thereof.

Background

The epoxy resin adhesive generally refers to an adhesive prepared by using epoxy resin as a main body. The epoxy resin has excellent chemical stability and corrosion resistance, good adhesive property, high mechanical strength and strong electrical insulation property, and is widely applied to industry.

The existing epoxy resin adhesive has high general hardness after being cured in order to meet the characteristics of chemical stability, corrosion resistance and the like, but the high hardness of the epoxy resin adhesive can cause the epoxy resin adhesive to have high brittleness and not have good toughness, so that the epoxy resin adhesive cannot meet the use requirements of some special occasions; in addition, the conventional epoxy resin adhesive composition often contains toxic materials, so that the epoxy resin adhesive is inconvenient for safe use in life.

Based on the formula, the invention designs a high-toughness and non-toxic epoxy resin adhesive formula and a preparation method thereof.

Disclosure of Invention

The invention aims to provide a formula of a high-toughness and non-toxic epoxy resin adhesive and a preparation method thereof, and aims to solve the problems that the conventional epoxy resin adhesive provided in the background art has high general hardness after curing in order to meet the characteristics of chemical stability, corrosion resistance and the like, but the high hardness can cause the epoxy resin adhesive to have high brittleness and not have good toughness, so that the epoxy resin adhesive cannot be used in some special occasions; in addition, the existing epoxy resin glue composition often contains toxic materials, so that the epoxy resin glue is inconvenient for safe use in life.

In order to achieve the purpose, the invention provides the following technical scheme: the formula of the high-toughness and non-toxic epoxy resin adhesive comprises the following raw material components in parts by weight:

as a further scheme of the invention, the mixed solvent is prepared by compounding ethanol and n-butanol according to the mass ratio of 8: 2.

As a further aspect of the present invention, the β -cyclodextrin complex is prepared by the following process: stirring beta-cyclodextrin, sodium hydroxide and pyridine, adding succinic anhydride, heating, stirring, adding dimethylformamide for crystallization, drying, adding sodium montmorillonite and water, stirring, adding tetradecyl tributyl ammonium chloride and dodecyl tributyl ammonium bromide, heating, stirring, filtering, washing solid with anhydrous ethanol, drying in air atmosphere, and pulverizing to obtain beta-cyclodextrin complex.

A preparation method of high-toughness and non-toxic epoxy resin adhesive comprises the following steps:

the first step is as follows: adding E-44 epoxy resin, beta-cyclodextrin compound, glass fiber powder and talcum powder into a reaction kettle, heating to 50-70 ℃, and stirring for 1-1.5 hours;

the second step is that: adding the mixed solvent and the curing agent into the mixture in the first step, and heating to

Stirring for 0.5-1 hour at 50-70 deg.C;

the third step: adding defoaming agent into the mixture of the second step, heating to 40-50 deg.c, stirring for 0.5-1 hr, cooling for 2-3 hr to room temperature and discharging.

Compared with the prior art, the invention has the beneficial effects that:

(1) the formula of the invention contains a beta-cyclodextrin compound, in the beta-cyclodextrin compound, the molecular shape of the beta-cyclodextrin is inner hydrophobic, the outer hydrophilic is slightly in a cone-cylinder-shaped cavity structure, the beta-cyclodextrin compound contains a large amount of primary hydroxyl and secondary hydroxyl, the beta-cyclodextrin compound is combined with succinic anhydride, the bonding degree is moderate, the water solubility is good, sodium-based montmorillonite can enter the cone-cylinder-shaped cavity of the beta-cyclodextrin, tetradecyl tributyl ammonium chloride and dodecyl tributyl ammonium bromide can enter the sodium-based montmorillonite to be exposed in the outer interlayer structure under certain conditions, so that the beta-cyclodextrin compound not only has high adsorption activity, but also has high bonding degree, and simultaneously the solubility with bisphenol S type epoxy resin and linear phenolic epoxy resin can be enhanced, the invention has excellent spreadability after curing, excellent bonding performance, and a hard segment with good heat resistance in the molecule, the adhesive has soft sections with good flexibility, small brittleness and obvious toughening effect;

(2) the formula of the epoxy resin adhesive contains the glass fiber powder, the glass fiber powder has good dispersibility of the powder and reinforcement of the chopped fibers, the hardness, the crack resistance of the product and the like can be obviously enhanced, and the stability of the epoxy resin adhesive can be improved;

(3) the formula of the epoxy resin adhesive contains the talcum powder, so that the tensile strength, the elongation and other characteristics of the epoxy resin adhesive can be improved, and the glossiness and the smoothness of the surface of the cured epoxy resin adhesive can be improved;

(4) the formula of the invention has no harmful components, and the use is safe and healthy.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic flow chart of the preparation method of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The invention provides a technical scheme that: the formula of the high-toughness and non-toxic epoxy resin adhesive comprises the following raw material components in parts by weight:

specifically, the mixed solvent is prepared by compounding ethanol and n-butanol according to the mass ratio of 8: 2.

Specifically, the beta-cyclodextrin compound is prepared by adopting the following process: stirring beta-cyclodextrin, sodium hydroxide and pyridine, adding succinic anhydride, heating, stirring, adding dimethylformamide for crystallization, drying, adding sodium montmorillonite and water, stirring, adding tetradecyl tributyl ammonium chloride and dodecyl tributyl ammonium bromide, heating, stirring, filtering, washing solid with anhydrous ethanol, drying in air atmosphere, and pulverizing to obtain beta-cyclodextrin complex.

Referring to fig. 1, a method for preparing a nontoxic epoxy resin adhesive with high toughness includes the following steps:

the first step is as follows: adding E-44 epoxy resin, beta-cyclodextrin compound, glass fiber powder and talcum powder into a reaction kettle, heating to 50-70 ℃, and stirring for 1-1.5 hours;

the second step is that: adding the mixed solvent and the curing agent into the mixture in the first step, heating to 50-70 ℃, and stirring for 0.5-1 hour;

the third step: adding defoaming agent into the mixture of the second step, heating to 40-50 deg.c, stirring for 0.5-1 hr, cooling for 2-3 hr to room temperature and discharging.

The formula of the invention contains beta-cyclodextrin compound, in the beta-cyclodextrin compound, the beta-cyclodextrin molecule is in a cavity structure with inner hydrophobicity and outer hydrophilicity in a cone cylinder shape, the beta-cyclodextrin compound contains a large amount of primary hydroxyl and secondary hydroxyl, the beta-cyclodextrin compound is combined with succinic anhydride, the bonding degree is moderate, the water solubility is good, sodium montmorillonite can enter the cone cylinder cavity of the beta-cyclodextrin, tetradecyl tributyl ammonium chloride and dodecyl tributyl ammonium bromide can enter the sodium montmorillonite to be exposed in the outer interlayer structure under a certain condition, the beta-cyclodextrin compound has high adsorption activity and bonding degree, the solubility with bisphenol S type epoxy resin and linear phenolic epoxy resin can be enhanced, the cured beta-cyclodextrin compound has excellent spreadability and bonding performance, the molecule of the beta-cyclodextrin compound has a hard segment with good heat resistance, but also has a soft segment with good flexibility, small brittleness of the adhesive and obvious toughening effect.

The glass fiber powder in the formula has good powder dispersibility and chopped fiber reinforcement, can obviously enhance the hardness, the crack resistance of products and the like, and can improve the stability of the epoxy resin adhesive; in addition, the talcum powder in the formula can improve the characteristics of the epoxy resin adhesive such as tensile strength, elongation and the like, and can improve the glossiness and smoothness of the surface of the cured epoxy resin adhesive; the formula of the invention has no harmful components, and the use is safe and healthy.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.