CN110922925B - Epoxy resin adhesive for wet surface of concrete - Google Patents
Epoxy resin adhesive for wet surface of concrete Download PDFInfo
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- CN110922925B CN110922925B CN201911187951.3A CN201911187951A CN110922925B CN 110922925 B CN110922925 B CN 110922925B CN 201911187951 A CN201911187951 A CN 201911187951A CN 110922925 B CN110922925 B CN 110922925B
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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
- 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
- C08G59/5006—Amines aliphatic
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- 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
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- 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
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
- C08G59/623—Aminophenols
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to an epoxy resin adhesive for a wet surface of concrete, and solves the problems of high cost, high brittleness, low toughness and further improvement of various performances of the conventional epoxy resin adhesive. The invention comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 2-4: 1, wherein the component A comprises the following raw materials in parts by weight: 100 parts of bisphenol A epoxy resin, 5-10 parts of palygorskite powder and 15-25 parts of waste glass powder; the component B comprises the following components in parts by weight: 45-65 parts of modified amine curing agent, 10-20 parts of monoamine and 4-6 parts of thixotropic agent. The invention has the advantages of simple raw materials, low cost, good flexibility, excellent hydrophobicity, low permeability, low toxicity, self-drying property and excellent bonding property, and is particularly suitable for wet surfaces of concrete.
Description
Technical Field
The invention relates to the field of adhesive preparation, in particular to an epoxy resin adhesive for a wet surface of concrete.
Background
Epoxy resin is a general name of a high molecular compound at least containing two epoxy groups, and because the epoxy groups have more active chemical activity and can react with various organic compounds and inorganic compounds, and meanwhile, the epoxy resin is a common thermosetting high molecular material, and the mechanical property, the adhesive property, the conductive property and the like of a cured product of the epoxy resin are different according to the type of a used curing agent, the epoxy resin can be widely used in the fields of adhesives, coatings, insulating materials, composite materials and the like.
Common curing agents are divided into two categories, namely heating curing agents and normal-temperature curing agents, the epoxy resin cured by heating is high in curing speed, but resources consumed by heating in the practical application process are large, the adhesive of the building waterproof coiled material generally mainly adopts a normal-temperature curing type or a low-temperature curing type, more curing agents are used, and the common normal-temperature curing agent, namely the phenolic amine curing agent, is high in tensile strength of a cured product due to large crosslinking density during curing, but the phenolic amine curing product is brittle and easy to longitudinally break due to large molecular weight of the phenolic amine.
In recent years, epoxy resin adhesives are used more in the field of building construction, but are influenced by weather such as rain and snow fall, common epoxy resin curing agents are high in water solubility, epoxy resin cannot be cured completely when the epoxy resin curing agents are used in a humid environment, the service life of a building can be shortened, particularly, due to the fact that the epoxy resin curing agents are used in rainy seasons in south China, self-adhesive waterproof coiled materials are used together with the adhesives in waterproof construction, but due to short construction period, waterproof construction sometimes has to be carried out on a low-temperature humid concrete surface, the common epoxy resin adhesives cannot be cured completely in the environment with low-temperature humidity or even a small amount of clear water, the waterproof coiled materials are not bonded firmly, and water seepage of the building is serious.
CN 105802566 discloses an epoxy resin series adhesive for CFRP (circulating fluidized bed) pasting on the surface of wet concrete, which combines two epoxy resin adhesives with different components, namely primer and impregnating adhesive, to prepare the epoxy resin series adhesive which can be cured within 1.5 hours at the normal temperature of the wet surface of a structure and reaches the use standard, and has stronger adhesive force and mechanical strength. The curing agent used in the invention is a T-31 curing agent, namely a commercially available phenolic aldehyde amine curing agent, although the curing agent can be cured in a humid environment, the cured adhesive has high brittleness and low toughness due to the excessively high molecular weight of the curing agent, and the adhesive is easy to longitudinally damage in the actual use process, so that the performance is invalid.
CN 102977830 discloses an epoxy resin adhesive, a preparation method and application thereof, the adhesive prepared by adding a toughening agent amino-terminated liquid nitrile rubber has good adhesive property and strong mechanical property, and is particularly suitable for being used as an adhesive layer of a vehicle composite material plate. Although the adhesive prepared by adding the nitrile rubber improves the bonding performance, the brittleness of the material is still not improved, and the liquid nitrile rubber has low domestic yield and high price and is not easy to produce in large quantities.
Disclosure of Invention
The invention aims to solve the technical problems and provide the epoxy resin adhesive for the wet surface of the concrete, which has the advantages of simple raw materials, low cost, good flexibility, excellent hydrophobicity, low permeability, low toxicity, self-drying property and excellent bonding property.
The epoxy resin adhesive for wet concrete surfaces is prepared from a component A and a component B, wherein the weight ratio of the component A to the component B is 2-4: 1, preferably 3:1, wherein the component A comprises the following raw materials in parts by weight: 100 parts of bisphenol A epoxy resin, 5-10 parts of palygorskite powder and 15-25 parts of waste glass powder; the component B comprises the following components in parts by weight: 45-65 parts of modified amine curing agent, 10-20 parts of monoamine and 4-6 parts of thixotropic agent.
The modified amine curing agent in the component B is prepared by the following method: the preparation method comprises the steps of carrying out Mannich (Mannich) reaction on 1, 6-hexanediamine, 37-40% of formaldehyde solution and cardanol, and then carrying out vacuum filtration.
The modified amine curing agent in the component B is prepared by the following method: mixing 116-174 parts of 1, 6-hexanediamine and 298-447 parts of cardanol, stirring, heating to 35-45 ℃, keeping for 0.5-1 h, heating to 70-80 ℃, slowly adding 60-90 parts of formaldehyde solution with the mass fraction of 37-40%, after the formaldehyde solution is added, heating to 90-100 ℃, keeping for 2-4 h for full reaction, vacuumizing, and filtering to obtain the modified amine curing agent. The palygorskite powder is prepared by taking palygorskite as a raw material and carrying out wet grinding, centrifugation, ultrasonic dispersion and drying.
The waste glass powder is superfine glass powder with the particle size of 200-800 mu m after wet grinding treatment.
The monoamine is at least one of isobutylamine or n-propylamine.
The thixotropic agent is white carbon black.
In view of the problems in the background art, the inventor makes the following improvements: (1) palygorskite powder and waste glass powder are added, the palygorskite powder with good adsorbability and filling property is used for replacing common epoxy resin filler modified montmorillonite, waste of energy resources is effectively reduced, the waste glass powder has the characteristics of high strength, high toughness and easiness in obtaining, the palygorskite powder is used as the filler for enhancing the water absorption and bonding strength of epoxy resin adhesives, waste utilization is facilitated, preferably, raw materials are subjected to wet grinding treatment, the raw materials can be ground to be finer by utilizing the wet grinding process, the original properties of the materials are protected due to the fact that the temperature in a bowl is lower than the temperature in a dry grinding bowl in the wet grinding, and the products after drying and filtering are pure and have fewer impurities; (2) the modified amine curing agent is prepared by taking 1, 6-hexamethylenediamine as a raw material, adding cardanol for reaction, then adding a formaldehyde solution, performing Mannich (Mannich) reaction, and then performing vacuum filtration, and the Mannich-modified amine curing agent is adopted, so that the toxicity of the curing agent is reduced, the activity of the amine curing agent is improved, the epoxy resin can be cured at normal temperature, low temperature and humid environment, cardanol is further used for replacing common phenol as a Mannich reactant, and the meta-position of cardanol hydroxyl group contains a carbon 15 straight chain with unsaturated double bonds, so that good flexibility, excellent hydrophobicity, low permeability and self-drying property of a system can be provided, and the cured product also has the advantage; in addition, compared with the phenol which is solid at normal temperature, the cardanol which is liquid at normal temperature is more beneficial to the full reaction. (3) Monoamine is added into the component B, and the monoamine has the characteristics of low price, easiness in obtaining, non-volatility at normal temperature and high reaction activity, can reduce the degree of crosslinking and curing, enables the epoxy resin adhesive to have stronger toughness, and solves the problem that the adhesive property of the epoxy resin adhesive is reduced due to overlarge molecular weight and overlarge brittleness. The addition amount of the monoamine is 10-20 parts, and if the monoamine is added too much, the curing efficiency of the curing agent is reduced and the curing is incomplete because the monoamine is an amine with small molecules and easy to dissolve in water; if the addition amount of the monoamine is too small, the average molecular weight of the whole curing agent is too large, the toughness of a cured product is reduced, and the brittleness is increased; the monoamine is preferably at least one of isobutylamine or n-propylamine.
Therefore, the epoxy resin adhesive obtained by selecting the proper filler, using the modified amine curing agent and simultaneously adding the monoamine has good flexibility, excellent hydrophobicity, low permeability, low toxicity, self-drying property and excellent bonding property, and is particularly suitable for wet surfaces of concrete; moreover, because the raw materials of each component are easy to obtain, the cost is further reduced, the batch production cost is possible, and the method has wide market application prospect.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) 5 parts of palygorskite subjected to wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 15 parts of glass powder subjected to dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) are mixed and fully stirred to obtain a component A.
2) Taking 116 parts of 1, 6-hexanediamine and 298 parts of cardanol, mixing, sequentially stirring and heating to 35 ℃ for 0.5h, heating to 70 ℃, slowly adding 60 parts of formaldehyde solution with the mass fraction of 37-40%, heating to 90 ℃ after the formaldehyde solution is dropwise added, keeping for 2h for sufficient reaction, vacuumizing and filtering to obtain a phenol-aldehyde-amine mixture, weighing 45 parts of phenol-aldehyde-amine mixture, mixing 10 parts of n-propylamine, 4 parts of white carbon black and the phenol-aldehyde-amine mixture, and stirring uniformly at normal temperature to obtain a component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 2:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
Example 2
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) 6.5 parts of palygorskite subjected to wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 17 parts of glass powder subjected to dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) are mixed and fully stirred to obtain the component A.
2) Mixing 130 parts of 1, 6-hexanediamine and 330 parts of cardanol, sequentially stirring and heating to 37 ℃ for 0.7h, heating to 75 ℃, slowly adding 70 parts of formaldehyde solution with the mass fraction of 37-40%, heating to 95 ℃ after the formaldehyde solution is dropwise added, keeping for 3h for sufficient reaction, vacuumizing and filtering to obtain a phenol-aldehyde-amine mixture, weighing 47 parts of the phenol-aldehyde-amine mixture, mixing 16 parts of n-propylamine, 5 parts of white carbon black and the phenol-aldehyde-amine mixture, and uniformly stirring at normal temperature to obtain a component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 2.5:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
Example 3
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) 8 parts of palygorskite subjected to wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 20 parts of glass powder subjected to dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) are mixed and fully stirred to obtain a component A.
2) Taking 141 parts of 1, 6-hexanediamine and 360 parts of cardanol, mixing, sequentially stirring and heating to 40 ℃ for 1h, heating to 80 ℃, slowly adding 75 parts of formaldehyde solution with the mass fraction of 37-40%, heating to 100 ℃ after the formaldehyde solution is dropwise added, keeping for 4h for sufficient reaction, vacuumizing and filtering to obtain a phenol-aldehyde-amine mixture, weighing 50 parts of the phenol-aldehyde-amine mixture, mixing 20 parts of n-propylamine and 6 parts of white carbon black with the phenol-aldehyde-amine mixture, and stirring uniformly at normal temperature to obtain a component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 3:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
Example 4
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) 8.5 parts of palygorskite after wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 23 parts of glass powder after dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) are mixed and fully stirred to obtain the component A.
2) 155 parts of 1, 6-hexanediamine and 400 parts of cardanol are mixed, sequentially stirred and heated to 36 ℃ for 0.5 hour, the mixture is heated to 70 ℃ and slowly added with 80 parts of formaldehyde solution with the mass fraction of 37-40%, after the formaldehyde solution is dropwise added, the mixture is heated to 90 ℃ for 2 hours for sufficient reaction, vacuum filtration is carried out to obtain a phenol-aldehyde-amine mixture, 55 parts of phenol-aldehyde-amine mixture is weighed, 10 parts of isobutylamine and 4 parts of white carbon black are mixed with the phenol-aldehyde-amine mixture, and the mixture is uniformly stirred at normal temperature to obtain the component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 3:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
Example 5
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) and mixing 9 parts of palygorskite subjected to wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 24 parts of glass powder subjected to dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) and fully stirring to obtain a component A.
2) Mixing 160 parts of 1, 6-hexanediamine and 420 parts of cardanol, sequentially stirring and heating to 43 ℃ for 0.7h, heating to 75 ℃, slowly adding 85 parts of formaldehyde solution with the mass fraction of 37-40%, heating to 95 ℃ after the formaldehyde solution is dropwise added, keeping for 3h for full reaction, vacuumizing and filtering to obtain a phenol-aldehyde-amine mixture, weighing 57 parts of phenol-aldehyde-amine mixture, mixing 18 parts of isobutylamine and 5 parts of white carbon black with the phenol-aldehyde-amine mixture, and uniformly stirring at normal temperature to obtain a component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 3.5:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
Example 6
An epoxy resin adhesive for concrete wet surfaces and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
1) 10 parts of palygorskite subjected to wet grinding, centrifugation, ultrasonic dispersion and drying treatment, 25 parts of glass powder subjected to dry grinding and wet grinding treatment and 100 parts of bisphenol A type epoxy resin (E-51) are mixed and fully stirred to obtain a component A.
2) Mixing 174 parts of 1, 6-hexanediamine and 447 parts of cardanol, sequentially stirring and heating to 45 ℃ for 1h, heating to 80 ℃, slowly adding 90 parts of formaldehyde solution with the mass fraction of 37-40%, heating to 100 ℃ after the formaldehyde solution is dropwise added, keeping for 4h for sufficient reaction, vacuumizing and filtering to obtain a phenalkamine mixture, weighing 65 parts of the phenalkamine mixture, mixing 20 parts of isobutylamine and 6 parts of white carbon black with the phenalkamine mixture, and uniformly stirring at normal temperature to obtain the component B.
And (3) fully mixing the component A and the component B according to the weight ratio of 4:1 at normal temperature to obtain the epoxy resin adhesive for the wet surface of concrete.
The data obtained by determining the impact test method of the resin casting body according to the standard GB/T2571-2008, the bending test method of the resin casting body according to the standard GB/T2567-2008 and the tensile shear strength of the adhesive according to the standard GB/T7124-2008 are shown in the following table 1
TABLE 1
As can be seen in the table, the epoxy resin adhesive has the advantages of good flexibility, excellent hydrophobicity, low permeability, low toxicity, self-drying property and excellent adhesive property, and is a good epoxy resin adhesive.
Claims (6)
1. The epoxy resin adhesive for wet concrete surfaces is characterized by being prepared by mixing a component A and a component B in a weight ratio of 2-4: 1, wherein the component A comprises the following raw materials in parts by weight: 100 parts of bisphenol A epoxy resin, 5-10 parts of palygorskite powder and 15-25 parts of waste glass powder; the component B comprises the following components in parts by weight: 45-65 parts of modified amine curing agent, 10-20 parts of monoamine and 4-6 parts of thixotropic agent;
the palygorskite powder is prepared by taking palygorskite as a raw material and carrying out wet grinding, centrifugation, ultrasonic dispersion and drying;
the modified amine curing agent in the component B is prepared by the following method: the formaldehyde solution is prepared by performing Mannich (Mannich) reaction on 116-174 parts by weight of 1, 6-hexanediamine, 60-90 parts by weight of formaldehyde solution with the mass fraction of 37% -40% and 298-447 parts by weight of cardanol, and then performing vacuum filtration.
2. The epoxy resin adhesive for wet concrete surfaces as claimed in claim 1, wherein the modified amine curing agent in the component B is prepared by the following method: mixing 116-174 parts by weight of 1, 6-hexanediamine and 298-447 parts by weight of cardanol, stirring, heating to 35-45 ℃, keeping for 0.5-1 h, heating to 70-80 ℃, slowly adding 60-90 parts by weight of formaldehyde solution with the mass fraction of 37-40%, after the formaldehyde solution is added, heating to 90-100 ℃, keeping for 2-4 h for full reaction, vacuumizing, and filtering to obtain the modified amine curing agent.
3. The epoxy resin adhesive for wet surfaces of concrete according to claim 1 or 2, wherein the waste glass powder is a wet-milled ultrafine glass powder with a particle size of 200-800 μm.
4. The epoxy adhesive for wet surfaces of concrete according to claim 1 or 2, wherein the monoamine is at least one of isobutylamine or n-propylamine.
5. The epoxy resin adhesive for wet concrete surfaces according to claim 1 or 2, wherein the thixotropic agent is white carbon black.
6. The epoxy resin adhesive for wet concrete surfaces according to claim 1 or 2, wherein the mixing weight ratio of the component A to the component B is 3: 1.
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| CN113527566A (en) * | 2021-07-21 | 2021-10-22 | 湖北工业大学 | Method for treating wet basal plane by using epoxy monomer modified aluminum sulfate cement |
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