CN113773758A - Instant adhesive and preparation method thereof - Google Patents
Instant adhesive and preparation method thereof Download PDFInfo
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- CN113773758A CN113773758A CN202111247095.3A CN202111247095A CN113773758A CN 113773758 A CN113773758 A CN 113773758A CN 202111247095 A CN202111247095 A CN 202111247095A CN 113773758 A CN113773758 A CN 113773758A
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- 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The invention provides an instant adhesive and a preparation method thereof. The instant adhesive is prepared from the following raw materials in parts by weight: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube. The invention also provides a preparation method of the instant adhesive. The instant adhesive has the advantages of strong water resistance, impact resistance, high temperature resistance and corrosion resistance, and has better binding power when being constructed in an aqueous medium.
Description
Technical Field
The invention relates to the technical field of chemical materials, in particular to an instant adhesive and a preparation method thereof.
Background
The existing instant adhesive has the advantages of wide bonding surface and strong bonding capability, and is considered to be one of the most important room temperature curing adhesives. However, the conventional instant adhesive has disadvantages of poor water resistance, impact resistance, high temperature resistance and corrosion resistance, and poor adhesion when applied in an aqueous medium.
Disclosure of Invention
The invention mainly aims to provide an instant adhesive which has strong water resistance, impact resistance, high temperature resistance and corrosion resistance and has better binding power when being constructed in an aqueous medium.
In order to solve the technical problems, the preparation raw materials of the instant adhesive provided by the invention comprise: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube.
Further, the thickening agent is at least one of methyl methacrylate-ethyl acrylate copolymer, polymethacrylate, polyvinyl acetate, polyacrylate, polyvinyl acetal and polyvinyl acetate; and/or
The organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and propylene carbonate.
Further, the preparation raw materials of the instant adhesive comprise, by weight: 0.05-0.3 part of plasticizer, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate.
Further, the preparation raw materials of the instant adhesive comprise, by weight: 0.1-0.3 part of first stabilizer, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide.
Further, the preparation raw materials of the instant adhesive comprise, by weight: 0.1-0.5 part of heat-resistant and water-resistant modifier, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride.
Further, the preparation raw materials of the instant adhesive also comprise: 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate.
The invention also provides a preparation method of the instant adhesive, which comprises the following steps:
providing 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube in parts by weight;
mixing the alpha-cyanoacrylate, the thickening agent and the organic solvent to obtain a mixture;
heating the mixture, and carrying out free radical polymerization reaction on the alpha-ethyl cyanoacrylate and the thickening agent to obtain a primary colloid;
carrying out reduced pressure distillation treatment on the primary colloid, and removing the organic solvent to obtain a colloid; and
and adding the graphene and the carbon nano tubes into a colloid, wherein the graphene and the carbon nano tubes form graphene/carbon nano tube aerogel and are uniformly dispersed in the colloid to prepare the instant drying adhesive.
Further, the thickening agent is at least one of methyl methacrylate-ethyl acrylate copolymer, polymethacrylate, polyvinyl acetate, polyacrylate, polyvinyl acetal and polyvinyl acetate; and/or
The organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and propylene carbonate.
Further, the preparation method of the instant adhesive further comprises the following steps:
providing 0.05-0.3 part of a plasticizer according to the parts by weight, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the plasticizer, and the organic solvent to obtain the mixture.
Further, the preparation method of the instant adhesive further comprises the following steps:
providing 0.1-0.3 parts of a first stabilizer by weight, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the first stabilizer, and the organic solvent to obtain the mixture.
Further, the preparation method of the instant adhesive further comprises the following steps:
providing 0.1-0.5 part of a heat-resistant and water-resistant modifier according to parts by weight, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride; and
mixing the alpha-ethyl cyanoacrylate, the thickening agent, the heat-resistant and water-resistant modifier and the organic solvent to obtain the mixture.
Further, after the initial colloid is obtained and before the graphene and the carbon nanotubes are added into the colloid, the preparation method of the instant drying adhesive further comprises the following steps:
providing 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler in parts by weight, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate; and
and adding the second stabilizer and the filler into the primary colloid, and carrying out reduced pressure distillation treatment on the second stabilizer, the filler and the primary colloid to obtain the colloid.
In the technical scheme of the invention, the preparation raw materials of the instant adhesive comprise, by weight: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube. The alpha-cyanoacrylate and the thickener can undergo radical polymerization to obtain colloid. The graphene and the carbon nanotubes can form graphene/carbon nanotube aerogel and be uniformly dispersed in the colloid. The graphene/carbon nanotube aerogel is very easy to be infiltrated by metal and forms a new metal-based composite material with a metal base material, so that the impact resistance, the peeling resistance and the high temperature resistance of the instant adhesive are improved. The graphene/carbon nanotube aerogel has a lamellar structure, a labyrinth shielding structure can be formed in the colloid, and the shielding structure can effectively inhibit infiltration, permeation and diffusion of corrosive media, so that the corrosion resistance of the instant adhesive is improved. Furthermore, the graphene/carbon nanotube aerogel also has a super-hydrophobic functional group, so that the water resistance of the instant adhesive can be improved, and the instant adhesive also has better binding power when constructed in an aqueous medium.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides an instant adhesive. The instant adhesive is a black, one-component adhesive.
The preparation raw materials of the instant adhesive comprise: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 0.05-0.3 part of a plasticizer, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube.
In at least one embodiment, the thickener is at least one of methyl methacrylate-ethyl acrylate copolymer, polymethacrylate, polyvinyl acetate, polyacrylate, polyvinyl acetal, and polyvinyl acetate. The thickener can undergo a free radical polymerization reaction with ethyl alpha-cyanoacrylate to increase the viscosity of the instant adhesive.
In at least one embodiment, the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, and dioctyl phthalate. The plasticizer weakens the physical effect of intermolecular forces in the polymer to provide the instant adhesive with better toughness and mechanical strength.
In at least one embodiment, the organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, and propylene carbonate.
As will be appreciated, the instant adhesive, when cured, becomes a tough elastomer with impact, heat, peel, corrosion, water resistance, etc. The instant adhesive can be used for bonding high-temperature resistant products such as loudspeaker parts, automobile elements, electronic equipment, oil filters, disk drives, server connectors and the like, can also be used for bonding products with waterproof and corrosion-resistant requirements, and can also be used for quickly and temporarily stopping leakage of metal ship hulls and wooden ship hulls in water media.
The instant adhesive provided by the technical scheme of the invention comprises the following raw materials in parts by weight: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube. And carrying out free radical polymerization reaction on the alpha-ethyl cyanoacrylate and the thickening agent to obtain the colloid. The graphene and the carbon nanotubes can form graphene/carbon nanotube aerogel and be uniformly dispersed in the colloid. The graphene/carbon nanotube aerogel is very easy to be infiltrated by a substrate such as a metal substrate and forms a new metal-based composite material with the metal substrate, so that the impact resistance, the peeling resistance and the high temperature resistance of the instant adhesive are improved. The graphene/carbon nanotube aerogel has a lamellar structure, a labyrinth shielding structure can be formed in the colloid, and the shielding structure can effectively inhibit infiltration, permeation and diffusion of corrosive media, so that the corrosion resistance of the instant adhesive is improved. Furthermore, the graphene/carbon nanotube aerogel also has a super-hydrophobic functional group, so that the water resistance of the instant adhesive can be improved, and the instant adhesive also has better binding power when constructed in an aqueous medium.
The instant adhesive is prepared from the following raw materials in parts by weight: 0.05-0.3 part of plasticizer, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate.
In the technical scheme of the invention, the raw materials for preparing the instant adhesive also comprise 0.05-0.3 part of plasticizer, and the plasticizer can weaken the physical action of intermolecular force of polymers so as to enable the instant adhesive to have better toughness and mechanical strength.
The instant adhesive is prepared from the following raw materials in parts by weight: 0.1-0.3 part of first stabilizer, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide.
In the technical scheme of the invention, the raw materials for preparing the instant adhesive also comprise 0.1-0.3 part of first stabilizer, and the first stabilizer can prevent the instant adhesive from undergoing anionic polymerization and free radical polymerization in the storage process.
The instant adhesive is prepared from the following raw materials in parts by weight: 0.1-0.5 part of heat-resistant and water-resistant modifier, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride.
In the technical scheme of the invention, the raw materials for preparing the instant adhesive also comprise 0.1-0.5 part of heat-resistant and water-resistant modifier, and the heat-resistant and water-resistant modifier can enable the instant adhesive to have better water resistance and heat resistance.
The instant adhesive is prepared from the following raw materials in parts by weight: 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate.
In the technical scheme of the invention, the preparation raw materials of the instant adhesive also comprise 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler. The second stabilizer may prevent anionic polymerization and free radical polymerization of the filler with the colloid. The filler may enhance the impact resistance of the instant adhesive.
In at least one preferred embodiment, the instant adhesive comprises, by weight, 60-70 parts of alpha-ethyl cyanoacrylate, 20-30 parts of a thickening agent, 0.05-0.3 part of a plasticizer, 1-3 parts of an organic solvent, 0.1-0.3 part of a first stabilizer, 0.6-0.8 part of a second stabilizer, 0.1-0.5 part of a heat-resistant and water-resistant modifier, 3-6 parts of a filler, 0.8-3 parts of graphene and 0.6-2 parts of a carbon nanotube.
The invention also provides a preparation method of the instant adhesive, which comprises the following steps:
providing 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 0.05-0.3 part of a plasticizer, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube in parts by weight;
mixing the alpha-cyanoacrylate, the thickening agent and the organic solvent to obtain a mixture;
heating the mixture, and carrying out free radical polymerization reaction on the alpha-ethyl cyanoacrylate and the thickening agent to obtain a primary colloid;
carrying out reduced pressure distillation treatment on the primary colloid to obtain a colloid; and
and adding the graphene and the carbon nano tubes into a colloid, wherein the graphene and the carbon nano tubes form graphene/carbon nano tube aerogel and are uniformly dispersed in the colloid to obtain the instant drying adhesive.
In at least one embodiment, the thickener is at least one of methyl methacrylate-ethyl acrylate copolymer, polymethacrylate, polyvinyl acetate, polyacrylate, polyvinyl acetal, and polyvinyl acetate.
In at least one embodiment, the organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, and propylene carbonate.
In at least one embodiment, the temperature of the heating treatment is 70-80 ℃ and the time is 30-120 min.
In at least one embodiment, the temperature of the reduced pressure distillation is 140-180 ℃.
According to the technical scheme, a mixture containing alpha-ethyl cyanoacrylate, a thickening agent and an organic solvent can be heated, the alpha-ethyl cyanoacrylate and the thickening agent are subjected to free radical polymerization to obtain a primary colloid, the primary colloid is subjected to reduced pressure distillation to obtain a clean colloid, graphene and carbon nanotubes are added into the colloid, and the graphene and the carbon nanotubes form graphene/carbon nanotube aerogel and are uniformly dispersed in the colloid to obtain the instant dry adhesive. The graphene/carbon nanotube aerogel is very easy to be infiltrated by metal and forms a new metal-based composite material with a metal base material, so that the impact resistance, the peeling resistance and the high temperature resistance of the instant adhesive are improved. The graphene/carbon nanotube aerogel has a lamellar structure, a labyrinth shielding structure can be formed in the colloid, and the shielding structure can effectively inhibit infiltration, permeation and diffusion of corrosive media, so that the corrosion resistance of the instant adhesive is improved. Furthermore, the graphene/carbon nanotube aerogel also has a super-hydrophobic functional group, so that the water resistance of the instant adhesive can be improved, and the instant adhesive also has better binding power when constructed in an aqueous medium.
The preparation method of the instant adhesive further comprises the following steps:
providing 0.05-0.3 part of a plasticizer according to the parts by weight, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the plasticizer, and the organic solvent to obtain the mixture.
In the technical scheme of the invention, the preparation method of the instant adhesive further comprises the step of mixing the alpha-cyanoacrylate, the thickening agent, the plasticizer and the organic solvent. The plasticizer weakens the physical effect of intermolecular forces in the polymer to provide the instant adhesive with better toughness and mechanical strength.
The preparation method of the instant adhesive further comprises the following steps:
providing 0.1-0.3 parts of a first stabilizer by weight, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the first stabilizer, and the organic solvent to obtain the mixture.
In the technical scheme of the invention, the preparation method of the instant adhesive further comprises the step of mixing the alpha-cyanoacrylate, the thickening agent, the first stabilizing agent and the organic solvent. The first stabilizer can prevent anionic polymerization and free radical polymerization of the instant adhesive during storage.
The preparation method of the instant adhesive further comprises the following steps:
providing 0.1-0.5 part of a heat-resistant and water-resistant modifier according to parts by weight, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride; and
mixing the alpha-ethyl cyanoacrylate, the thickening agent, the heat-resistant and water-resistant modifier and the organic solvent to obtain the mixture.
In the technical scheme of the invention, the preparation method of the instant adhesive further comprises the step of mixing the alpha-cyanoacrylate, the thickening agent, the heat-resistant and water-resistant modifier and the organic solvent. The heat-resistant and water-resistant modifier can enable the instant adhesive to have better water resistance and heat resistance.
After the primary colloid is obtained and before the graphene and the carbon nanotubes are added into the colloid, the preparation method of the instant adhesive further comprises the following steps:
providing 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler in parts by weight, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate; and
and adding the second stabilizer and the filler into the primary colloid, and carrying out reduced pressure distillation treatment on the second stabilizer, the filler and the primary colloid to obtain the colloid.
In the technical scheme of the invention, the preparation method of the instant adhesive further comprises the steps of adding the second stabilizer and the filler into the initial colloid, and carrying out reduced pressure distillation treatment on the second stabilizer, the filler and the initial colloid. The second stabilizer may prevent anionic polymerization and free radical polymerization of the filler with the colloid. The filler may enhance the impact resistance of the instant adhesive. By the reduced pressure distillation treatment, a clean colloid can be obtained.
The present invention will be specifically described below with reference to specific examples.
The first embodiment is as follows:
providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 78.5 parts of alpha-ethyl cyanoacrylate, 10.2 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.1 part of benzophenone tetracarboxylic dianhydride, 4.2 parts of silicon dioxide, 2 parts of graphene and 3 parts of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the first embodiment.
The instant adhesive of example one had a black appearance and a viscosity of 1000 pa.s.
Example two
Providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 74.6 parts of alpha-ethyl cyanoacrylate, 14.1 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.1 part of benzophenone tetracarboxylic dianhydride, 4.2 parts of silicon dioxide, 3 parts of graphene and 2 parts of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the second embodiment.
The instant adhesive of example two had a black appearance and a viscosity of 3000 pa.s.
EXAMPLE III
Providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 71.8 parts of alpha-ethyl cyanoacrylate, 17 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.2 part of benzophenone tetracarboxylic dianhydride, 5 parts of silicon dioxide, 1.5 parts of graphene and 2.5 parts of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and (3) uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the third embodiment.
The instant adhesive of example three had a black appearance and a viscosity of 5000 pa.s.
Example four
Providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 67.8 parts of alpha-ethyl cyanoacrylate, 21 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.2 part of benzophenone tetracarboxylic dianhydride, 5 parts of silicon dioxide, 2.5 parts of graphene and 1.5 parts of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and (3) uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the fourth embodiment.
The instant adhesive of example four had a black appearance and a viscosity of 8000 pa.s.
EXAMPLE five
Providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 64.5 parts of alpha-ethyl cyanoacrylate, 25.4 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.1 part of benzophenone tetracarboxylic dianhydride, 5 parts of silicon dioxide, 2 parts of graphene and 1 part of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and (3) uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the fifth embodiment.
The instant adhesive of example five had a black appearance and a viscosity of 10000 pa.s.
EXAMPLE six
Providing raw materials for preparing the instantaneous dry adhesive of the first embodiment, wherein the raw materials for preparing the instantaneous dry adhesive of the first embodiment comprise the following components in parts by weight: 55.5 parts of alpha-ethyl cyanoacrylate, 36.4 parts of methyl methacrylate-ethyl acrylate copolymer, 0.2 part of dioctyl ester, 1 part of ethylene carbonate, 0.2 part of sulfur dioxide, 0.6 part of hydroquinone, 0.1 part of benzophenone tetracarboxylic dianhydride, 3 parts of silicon dioxide, 1 part of graphene and 2 parts of carbon nano tube;
adding alpha-ethyl cyanoacrylate, methyl methacrylate-ethyl acrylate copolymer, dioctyl ester, ethylene carbonate, sulfur dioxide and benzophenone tetracarboxylic dianhydride into a reaction kettle, uniformly mixing, and reacting at the temperature of 70-80 ℃ for 120min to obtain a primary colloid;
adding hydroquinone and silicon dioxide into the primary colloid, and then distilling at 140 ℃ under reduced pressure to remove the organic solvent to obtain colloid; and
and uniformly stirring the graphene and the carbon nanotubes in the colloid to obtain the instantaneous-drying adhesive of the sixth embodiment.
The instant adhesive of example six had a black appearance and a viscosity of 18000 pa.s.
Steel test pieces were bonded using the instant adhesive of examples one to six, cured at a temperature of 22 ℃ for 16After 8h, the shear strength of the instant adhesive of examples one to six was tested to 26.4N/mm, respectively2、26.7N/mm2、26.3N/mm2、26.5N/mm2、26.6N/mm2、21.6N/mm2. This indicates. The instant dry adhesives of examples one to six had better tack and impact resistance.
The steel test pieces are bonded by using the instant dry adhesives of the first to the sixth examples, and after the steel test pieces are placed in a constant temperature and humidity box with the temperature of 120 ℃ for 72 hours, the shear strength of the instant dry adhesives of the first to the sixth examples is tested to be 24.8N/mm2、25.2N/mm2、24.2N/mm2、24.6N/mm2、25.3N/mm2、21.5N/mm2. This indicates. The instant dry adhesives of examples one to six have better high temperature resistance.
The steel test pieces were bonded using the adhesives of examples one to six, cured at 22 ℃ for 24 hours, subjected to a neutral salt spray test, and then tested to give the adhesives of examples one to six having shear strengths of 23.5N/mm, respectively2、23.8N/mm2、23.3N/mm2、23.5N/mm2、23.7N/mm2、21.2N/mm2. This indicates. The instant dry adhesives of examples one to six have better corrosion resistance.
The steel test pieces were bonded using the instant adhesives of examples one to six, cured at 22 ℃ for 24 hours, subjected to IP68 water resistance test, and then tested to obtain shear strengths of the instant adhesives of examples one to six of 25.1N/mm, respectively2、25.3N/mm2、25.0N/mm2、25.2N/mm2、25.4N/mm2、20.8N/mm2. This indicates. The instant adhesive of embodiments one to six has better water resistance.
The steel test pieces were bonded in an aqueous medium using the instant adhesives of examples one to six, and after curing at a temperature of 22 ℃ for 24 hours, the shear strengths of the instant adhesives of examples one to six were tested to be 12.3N/mm, respectively2、12.8.0N/mm2、16.0N/mm2、16.8N/mm2、22.1N/mm2、13.2N/mm2. This demonstrates the instantaneous stem of embodiments one through sixThe adhesive also has better binding power when constructed in an aqueous medium.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which can be directly or indirectly applied to other related technical fields without departing from the spirit of the present invention, are included in the scope of the present invention.
Claims (12)
1. The instant adhesive is characterized by comprising the following raw materials in parts by weight: 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube.
2. The adhesive of claim 1, wherein the thickener is at least one of a methyl methacrylate-ethyl acrylate copolymer, a polymethacrylate, a polyvinyl acetate, a polyacrylate, a polyvinyl acetal, and a polyvinyl acetate; and/or
The organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and propylene carbonate.
3. The adhesive of claim 1, wherein the adhesive is prepared from the following raw materials in parts by weight: 0.05-0.3 part of plasticizer, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate.
4. The adhesive of claim 1, wherein the adhesive is prepared from the following raw materials in parts by weight: 0.1-0.3 part of first stabilizer, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide.
5. The adhesive of claim 1, wherein the adhesive is prepared from the following raw materials in parts by weight: 0.1-0.5 part of heat-resistant and water-resistant modifier, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride.
6. The adhesive of claim 1 wherein the adhesive is prepared from the following raw materials: 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate.
7. A method for preparing an instantaneous adhesive, characterized in that it comprises the following steps:
providing 55-80 parts of alpha-ethyl cyanoacrylate, 10-40 parts of a thickening agent, 1-3 parts of an organic solvent, 0.5-5 parts of graphene and 0.5-5 parts of a carbon nano tube in parts by weight;
mixing the alpha-cyanoacrylate, the thickening agent and the organic solvent to obtain a mixture;
heating the mixture, and carrying out free radical polymerization reaction on the alpha-ethyl cyanoacrylate and the thickening agent to obtain a primary colloid;
carrying out reduced pressure distillation treatment on the primary colloid, and removing the organic solvent to obtain a colloid; and
and adding the graphene and the carbon nano tubes into a colloid, wherein the graphene and the carbon nano tubes form graphene/carbon nano tube aerogel and are uniformly dispersed in the colloid to prepare the instant drying adhesive.
8. The method of claim 7, wherein the thickener is at least one of methyl methacrylate-ethyl acrylate copolymer, polymethacrylate, polyvinyl acetate, polyacrylate, polyvinyl acetal, and polyvinyl acetate; and/or
The organic solvent is at least one of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate and propylene carbonate.
9. The method of making an adhesive according to claim 7, wherein the method of making an adhesive further comprises the steps of:
providing 0.05-0.3 part of a plasticizer according to the parts by weight, wherein the plasticizer is at least one of dioctyl phthalate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the plasticizer, and the organic solvent to obtain the mixture.
10. The method of making an adhesive according to claim 7, wherein the method of making an adhesive further comprises the steps of:
providing 0.1-0.3 parts of a first stabilizer by weight, wherein the first stabilizer is at least one of sulfur dioxide, p-toluenesulfonic acid, methanesulfonic acid, propane sultone and phosphorus pentoxide; and
mixing the ethyl alpha-cyanoacrylate, the thickener, the first stabilizer, and the organic solvent to obtain the mixture.
11. The method of making an adhesive according to claim 7, wherein the method of making an adhesive further comprises the steps of:
providing 0.1-0.5 part of a heat-resistant and water-resistant modifier according to parts by weight, wherein the heat-resistant and water-resistant modifier is at least one of benzophenone tetracarboxylic dianhydride and maleic anhydride; and
mixing the alpha-ethyl cyanoacrylate, the thickening agent, the heat-resistant and water-resistant modifier and the organic solvent to obtain the mixture.
12. The method of preparing an instant adhesive according to claim 7, wherein after the initial colloid is obtained and before the graphene and the carbon nanotubes are added to the colloid, the method further comprises the steps of:
providing 0.6-0.8 part of a second stabilizer and 2-8 parts of a filler in parts by weight, wherein the second stabilizer is at least one of quinone, hydroquinone, p-methoxyphenol and hindered phenol, and the filler is at least one of silicon dioxide, aluminum oxide and calcium carbonate; and
and adding the second stabilizer and the filler into the primary colloid, and carrying out reduced pressure distillation treatment on the second stabilizer, the filler and the primary colloid to obtain the colloid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111247095.3A CN113773758A (en) | 2021-10-26 | 2021-10-26 | Instant adhesive and preparation method thereof |
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| CN202111247095.3A CN113773758A (en) | 2021-10-26 | 2021-10-26 | Instant adhesive and preparation method thereof |
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| CN113773758A true CN113773758A (en) | 2021-12-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395334A (en) * | 2022-03-15 | 2022-04-26 | 宁波百仕高联合工业有限公司 | Preparation method of high-water-resistance instant adhesive |
| CN116731666A (en) * | 2023-08-15 | 2023-09-12 | 山东凯恩新材料科技有限公司 | Waterproof quick-drying adhesive and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666293A (en) * | 2013-12-02 | 2014-03-26 | 南通瑞普埃尔生物工程有限公司 | Heat resistance instant dry adhesive and preparation method thereof |
| CN109461937A (en) * | 2018-10-19 | 2019-03-12 | 深圳市优宝新材料科技有限公司 | A kind of lithium battery three-dimensional hybrid conductive adhesive and include the battery of the binder |
-
2021
- 2021-10-26 CN CN202111247095.3A patent/CN113773758A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666293A (en) * | 2013-12-02 | 2014-03-26 | 南通瑞普埃尔生物工程有限公司 | Heat resistance instant dry adhesive and preparation method thereof |
| CN109461937A (en) * | 2018-10-19 | 2019-03-12 | 深圳市优宝新材料科技有限公司 | A kind of lithium battery three-dimensional hybrid conductive adhesive and include the battery of the binder |
Non-Patent Citations (1)
| Title |
|---|
| 李子东 等: "《现代胶粘技术手册》", 31 January 2002, 新时代出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395334A (en) * | 2022-03-15 | 2022-04-26 | 宁波百仕高联合工业有限公司 | Preparation method of high-water-resistance instant adhesive |
| CN114395334B (en) * | 2022-03-15 | 2023-09-26 | 宁波百仕高联合工业有限公司 | Preparation method of high-water-resistance instant adhesive |
| CN116731666A (en) * | 2023-08-15 | 2023-09-12 | 山东凯恩新材料科技有限公司 | Waterproof quick-drying adhesive and preparation method thereof |
| CN116731666B (en) * | 2023-08-15 | 2023-10-20 | 山东凯恩新材料科技有限公司 | Waterproof quick-drying adhesive and preparation method thereof |
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Application publication date: 20211210 |