CN111876115A - Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof - Google Patents
Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof Download PDFInfo
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- CN111876115A CN111876115A CN202010832897.XA CN202010832897A CN111876115A CN 111876115 A CN111876115 A CN 111876115A CN 202010832897 A CN202010832897 A CN 202010832897A CN 111876115 A CN111876115 A CN 111876115A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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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- 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
- C09J11/06—Non-macromolecular additives organic
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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
- C09J11/08—Macromolecular additives
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- 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
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- 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
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an organic silicon modified high-temperature-resistant epoxy structural adhesive and a preparation method thereof, and belongs to the technical field of structural adhesives. The structural adhesive is prepared from the following raw materials in percentage by mass: 25-40 Wt% of organic silicon modified epoxy resin and 3-10 Wt% of organic silicon resin; 20-25 Wt% of aromatic amine; epoxy active diluent, 8-15 Wt%, amorphous silicon dioxide 20-28 Wt%, and assistant 0.5-2 Wt%. The organic silicon modified epoxy resin has high heat resistance, the thermal deformation temperature of the organic silicon modified epoxy resin is much higher than that of other epoxy resins, the aromatic amine curing agent can be cured at normal temperature and can resist high temperature, and an auxiliary agent is added; the whole epoxy structural adhesive has better high temperature resistance, the direct addition of the auxiliary agent solves the problems of poor wettability and dispersibility of the epoxy resin, the wettability and the dispersibility are good, the bonding force between the epoxy structural adhesive and an epoxy resin matrix is enhanced, and the high temperature resistance of the epoxy structural adhesive is more effectively exerted.
Description
Technical Field
The invention belongs to the technical field of structural adhesives, and particularly relates to an organic silicon modified high-temperature-resistant epoxy structural adhesive and a preparation method thereof.
Background
The structural adhesive is a building adhesive taking a high-molecular synthetic material as a main component, and the main type of the structural adhesive is an epoxy resin adhesive. The structural adhesive has the characteristics of large cohesion after curing and high bonding strength. The construction structure glue is mainly used for high-strength and quick fixing of equipment anchor bolts, embedded parts for bonding and connecting concrete, tie bars, granite decorative stone sheets and marble wall surfaces, repairing runways, leaking stoppage and the like, and is mainly used for maintenance and reinforcement of a lost or unreduced reinforced concrete structure, foundation construction of special building structures, bridge piles, reinforcement and maintenance of high-rise buildings and highway bridges and the like. The common epoxy resin adhesive cannot resist high temperature, so that the common epoxy resin adhesive cannot be used in high-temperature occasions and the application range of the common epoxy resin adhesive is limited, and therefore, aiming at the problems, the organic silicon modified high-temperature-resistant epoxy structural adhesive and the preparation method thereof have important significance.
Disclosure of Invention
The invention provides an organic silicon modified high-temperature-resistant epoxy structural adhesive and a preparation method thereof, and solves the problems.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to an organic silicon modified high-temperature-resistant epoxy structural adhesive which is prepared from the following raw materials in percentage by mass:
further, the organic silicon modified epoxy resin is prepared by the following steps: dissolving epoxy resin and organic silicon resin in a mixed solvent of dimethylbenzene and butyl acetate, adding a catalyst after the epoxy resin and the organic silicon resin are completely dissolved, heating and refluxing, controlling the temperature and time of reflux reaction, and carrying out reduced pressure distillation after the reaction is finished to obtain the clear and transparent organic silicon modified epoxy resin.
Further, the silicone resin can be any one or more of, but not limited to, a polymethylsilicon resin, a polyarylsilicone resin, and a polyalkylarylsilicone resin.
Further, the auxiliary agent comprises the following components: dispersing agent: 10-15 parts of wetting agent: 2-6 parts of curing agent, 20-50 parts of flatting agent: 2-6 parts of a film-forming assistant: 5-10 parts of a thickening agent: 5-10 parts of hydroxyethyl cellulose: 5-10 parts of a pH regulator: 1-5 parts of a silane coupling agent: 40-60 parts;
the dispersing agent is one or more of hydrophobic modified carboxylic acid sodium salt, polyacrylic acid sodium salt or ammonium salt; the flatting agent is modified polyester acrylate; the film-forming additive is prepared from glycol decaether and dipropylene glycol butyl ether according to the following weight percentage: the dipropylene glycol butyl ether is compounded in the weight ratio of 1: 1; the thickener comprises: one or more of diatomite, sodium bentonite, polyurethane, polyvinyl alcohol or polyacrylamide; the curing agent is one of diethylenetriamine, m-phenylenediamine, DMP-30/polyamide 650, phenolic aldehyde modified amine and diaminodiphenyl methane sulfone DDS.
A preparation method of an organic silicon modified high-temperature-resistant epoxy structural adhesive comprises the following steps:
s1, grinding: grinding the amorphous silicon dioxide and the auxiliary agent together to powder in percentage by mass;
s2, mixing: placing the organic silicon modified epoxy resin, the organic silicon resin, the aromatic amine, the epoxy active diluent, the ground amorphous silicon dioxide and the auxiliary agent powder in the raw materials in percentage by mass into a stirrer for mixing;
s3, stirring: placing the mixed raw materials in a stirrer, stirring at the speed of 300r/min for 30min, and standing;
s4, filtering: standing the mixed solution for 5min after stirring to obtain a finished product of the organic silicon modified high-temperature-resistant epoxy structural adhesive;
s5, packaging: and barreling and packaging the filtered finished product glue.
Compared with the prior art, the invention has the following beneficial effects:
the organic silicon modified epoxy resin has high heat resistance, the thermal deformation temperature is much higher than that of other epoxy resins, the aromatic amine curing agent can be cured at normal temperature and can resist high temperature, and an auxiliary agent is added. The whole epoxy structural adhesive has better high temperature resistance, and the direct addition of the auxiliary agent solves the problem of poor wettability and dispersibility of the epoxy resin, so that the organic silicon modified high temperature resistant epoxy structural adhesive has good wettability and dispersibility, enhances the bonding force with an epoxy resin matrix, and more effectively exerts the high temperature resistance.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
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 process diagram of the preparation method of the organic silicon modified high temperature resistant epoxy structural adhesive.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Example 1:
the invention relates to an organic silicon modified high-temperature-resistant epoxy structural adhesive which is prepared from the following raw materials in percentage by mass:
the organic silicon modified epoxy resin is prepared by the following steps: dissolving epoxy resin and organic silicon resin in a mixed solvent of dimethylbenzene and butyl acetate, adding a catalyst after the epoxy resin and the organic silicon resin are completely dissolved, heating and refluxing, controlling the temperature and time of a reflux reaction, and performing reduced pressure distillation after the reaction is finished to obtain clear and transparent organic silicon modified epoxy resin; the catalyst is titanium acetylacetonate.
The organic silicon resin is any one or more of, but not limited to, polymethyl silicon resin, polyaryl organic silicon resin and polyalkyl aryl organic silicon resin.
Wherein, the auxiliary agent comprises the following components: dispersing agent: 10 parts, wetting agent: 6 parts, 20 parts of curing agent, and a flatting agent: 4 parts of a film-forming additive: 5 parts of a thickening agent: 5 parts, hydroxyethyl cellulose: 5 parts, pH regulator: 5 parts, silane coupling agent: 40 parts of a mixture;
the dispersing agent is one or more of hydrophobic modified carboxylic acid sodium salt, polyacrylic acid sodium salt or ammonium salt; the flatting agent is modified polyester acrylate; the film forming additive is decaglycol ester and dipropylene glycol butyl ether according to the weight ratio of decaglycol ester: the dipropylene glycol butyl ether is compounded in the weight ratio of 1: 1; the thickening agent comprises: one or more of diatomite, sodium bentonite, polyurethane, polyvinyl alcohol or polyacrylamide; the curing agent is one of diethylenetriamine, m-phenylenediamine, DMP-30/polyamide 650, phenolic aldehyde modified amine and diaminodiphenyl methane sulfone DDS.
As shown in fig. 1, a preparation method of an organosilicon modified high temperature resistant epoxy structural adhesive comprises the following steps:
s1, grinding: grinding amorphous silicon dioxide and an auxiliary agent together by mass percent into powder;
s2, mixing: placing organic silicon modified epoxy resin, organic silicon resin, aromatic amine, epoxy active diluent, ground amorphous silicon dioxide and auxiliary agent powder in a stirrer for mixing according to mass percentage;
s3, stirring: placing the mixed raw materials in a stirrer, stirring at the speed of 300r/min for 30min, and standing;
s4, filtering: standing the mixed solution for 5min after stirring to obtain a finished product of the organic silicon modified high-temperature-resistant epoxy structural adhesive;
s5, packaging: and barreling and packaging the filtered finished product glue.
Example 2:
the organic silicon modified high-temperature-resistant epoxy structural adhesive of the embodiment is different from 1 of embodiment 1 in that the structural adhesive is prepared from the following raw materials in percentage by mass:
wherein, the auxiliary agent comprises the following components: dispersing agent: 15 parts, wetting agent: 2 parts, 22 parts of curing agent, and delustering agent: 4 parts of a film-forming additive: 6 parts of a thickening agent: 5 parts, hydroxyethyl cellulose: 5 parts, pH regulator: 1 part, silane coupling agent: 40 parts of the components.
The beneficial effects of the invention include but are not limited to:
the organic silicon modified epoxy resin has high heat resistance, the thermal deformation temperature is much higher than that of other epoxy resins, the aromatic amine curing agent can be cured at normal temperature and can resist high temperature, and an auxiliary agent is added. The whole epoxy structural adhesive has better high temperature resistance, and the direct addition of the auxiliary agent solves the problem of poor wettability and dispersibility of the epoxy resin, so that the organic silicon modified high temperature resistant epoxy structural adhesive has good wettability and dispersibility, enhances the bonding force with an epoxy resin matrix, and more effectively exerts the high temperature resistance.
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.
Claims (5)
1. The organic silicon modified high-temperature-resistant epoxy structural adhesive is characterized by being prepared from the following raw materials in percentage by mass:
2. the organic silicon modified high temperature resistant epoxy structural adhesive according to claim 1, wherein the organic silicon modified epoxy resin is prepared by the following steps: dissolving epoxy resin and organic silicon resin in a mixed solvent of dimethylbenzene and butyl acetate, adding a catalyst after the epoxy resin and the organic silicon resin are completely dissolved, heating and refluxing, controlling the temperature and time of reflux reaction, and carrying out reduced pressure distillation after the reaction is finished to obtain the clear and transparent organic silicon modified epoxy resin.
3. The silicone-modified high-temperature-resistant epoxy structural adhesive as claimed in claim 1, wherein the silicone resin includes but is not limited to any one or more of a polymethylsilicon resin, a polyarylsilicone resin, and a polyalkylarylsilicone resin.
4. The organic silicon modified high-temperature-resistant epoxy structural adhesive as claimed in claim 1, wherein the auxiliary agent comprises the following components: dispersing agent: 10-15 parts of wetting agent: 2-6 parts of curing agent, 20-50 parts of flatting agent: 2-6 parts of a film-forming assistant: 5-10 parts of a thickening agent: 5-10 parts of hydroxyethyl cellulose: 5-10 parts of a pH regulator: 1-5 parts of a silane coupling agent: 40-60 parts;
the dispersing agent is one or more of hydrophobic modified carboxylic acid sodium salt, polyacrylic acid sodium salt or ammonium salt; the flatting agent is modified polyester acrylate; the film-forming additive is prepared from glycol decaether and dipropylene glycol butyl ether according to the following weight percentage: the dipropylene glycol butyl ether is compounded in the weight ratio of 1: 1; the thickener comprises: one or more of diatomite, sodium bentonite, polyurethane, polyvinyl alcohol or polyacrylamide; the curing agent is one of diethylenetriamine, m-phenylenediamine, DMP-30/polyamide 650, phenolic aldehyde modified amine and diaminodiphenyl methane sulfone DDS.
5. The preparation method of the organic silicon modified high temperature resistant epoxy structural adhesive as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
s1, grinding: grinding the amorphous silicon dioxide and the auxiliary agent together to powder in percentage by mass;
s2, mixing: placing the organic silicon modified epoxy resin, the organic silicon resin, the aromatic amine, the epoxy active diluent, the ground amorphous silicon dioxide and the auxiliary agent powder in the raw materials in percentage by mass into a stirrer for mixing;
s3, stirring: placing the mixed raw materials in a stirrer, stirring at the speed of 300r/min for 30min, and standing;
s4, filtering: standing the mixed solution for 5min after stirring to obtain a finished product of the organic silicon modified high-temperature-resistant epoxy structural adhesive;
s5, packaging: and barreling and packaging the filtered finished product glue.
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| CN202010832897.XA CN111876115A (en) | 2020-08-18 | 2020-08-18 | Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof |
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| CN202010832897.XA CN111876115A (en) | 2020-08-18 | 2020-08-18 | Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof |
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