CN115029090A - High-thixotropy modified epoxy resin steel adhesive and preparation method thereof - Google Patents

High-thixotropy modified epoxy resin steel adhesive and preparation method thereof Download PDF

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Publication number
CN115029090A
CN115029090A CN202210764921.XA CN202210764921A CN115029090A CN 115029090 A CN115029090 A CN 115029090A CN 202210764921 A CN202210764921 A CN 202210764921A CN 115029090 A CN115029090 A CN 115029090A
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China
Prior art keywords
parts
component
epoxy resin
modified epoxy
steel adhesive
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CN202210764921.XA
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Chinese (zh)
Inventor
董连成
王东阳
王同帅
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Kehui Henan New Material Technology Co ltd
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Kehui Henan New Material Technology Co ltd
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Priority to CN202210764921.XA priority Critical patent/CN115029090A/en
Publication of CN115029090A publication Critical patent/CN115029090A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to the technical field of engineering materials, and discloses a high thixotropic modified epoxy resin steel adhesive which comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 80-100 parts of epoxy resin, 7-14 parts of liquid nitrile rubber, 4-10 parts of alkyl glycidyl ether and 80-145 parts of active light calcium carbonate. According to the high-thixotropy modified epoxy resin steel-sticking adhesive and the preparation method thereof, the tensile strength of a colloid can be greatly improved through modification of filler bentonite, the shear strength of the colloid can be greatly improved through doping of nano silica, although the tensile strength can be reduced to some extent, the influence of the bonding surface condition (smoothness) of a bonding surface on the bonding performance is large, the smoother the bonding surface is, the colloid is better in bonding performance, and the modified bentonite and the nano silica act simultaneously, so that the colloid has good stability in tensile strength and bonding performance.

Description

High-thixotropy modified epoxy resin steel adhesive and preparation method thereof
Technical Field
The invention relates to the technical field of engineering materials, in particular to a high thixotropic modified epoxy resin steel adhesive and a preparation method thereof.
Background
In the last 80 th century, until now, structural adhesives are applied to bridge reinforcement to obtain a certain effect, most of base materials used by the structural adhesives are epoxy resin high-molecular compounds with relatively good aging resistance, the initial bonding strength is high, the effect is good, the requirements of design and construction in various aspects can be met, but the bonding strength of the structural and steel plate interface needs to be improved, and the steel bonding adhesive serving as a steel bonding reinforcement material becomes a hotspot concerned by researchers.
The epoxy steel adhesive is one kind of building structural adhesive, is mainly applied to foundation engineering and reinforcing of bearing parts, is an important component of the building structural adhesive, has important function and wide application, is a structural adhesive prepared by mainly using epoxy resin as a main material and adding functional additives and fillers, has good processing and construction performance, has good chemical stability, strong acid and alkali resistance and a wide application range, but has relatively high price, and is added with a plurality of other materials in order to reduce cost in enterprise production, so that the mechanical property and the construction performance of the steel adhesive are reduced, and the popularization and the application of the steel adhesive are influenced.
In the preparation process of the epoxy resin adhesive, the filler is used to reduce the cost of the composite material, but the filler has more complex action than the cost reduction, and the filler is properly used to improve the processing technology performance of a resin system and the performance of a cured product, such as thixotropy, reduction of curing shrinkage, increase of compressive strength, hardness increase, electrical performance improvement and the like.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the high thixotropic modified epoxy resin steel adhesive and the preparation method thereof, which have the advantages of stable bonding performance and the like and solve the problem of unstable bonding performance.
(II) technical scheme
In order to achieve the purpose of instable bonding performance, the invention provides the following technical scheme: the high thixotropic modified epoxy resin steel adhesive comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 80-100 parts of epoxy resin, 7-14 parts of liquid nitrile rubber, 4-10 parts of alkyl glycidyl ether, 80-145 parts of active light calcium carbonate, 30-40 parts of active filler and 10-15 parts of toughening agent; the component B comprises the following components in parts by mass: 10-20 parts of wetting agent, 5-10 parts of CTAB modified bentonite, 15-30 parts of talcum powder, 1-5 parts of coupling agent, 15-30 parts of nano silicon dioxide, 1-3 parts of curing agent (1) and 10-20 parts of polymer.
Preferably, the active filler is active silica micropowder, the polymer is polyacrylate, and the toughening agent is a mixture with different active end groups and different types of chain segments connected through ester bonds or urethane bonds.
Preferably, the wetting agent is sulfonated oil, the curing agent (1) is polyisocyanate, the component C is 25-35 parts of the curing agent (2), and the curing agent (2) is low-molecular polyamide.
Preferably, the epoxy resin is bisphenol A diglycidyl ether, and the coupling agent is methacryloxypropyltrimethoxysilane, which is an organofunctional silane coupling agent.
The invention provides a preparation method of high thixotropic modified epoxy resin steel adhesive, which comprises the following steps:
1) preparation: weighing 8-10g of modifier, adding the modifier into a 1000mL beaker, adding 792mL of deionized water, heating and stirring until the solid is dissolved, adding 80g of bentonite when the water temperature is constant at 84 ℃, stirring at constant temperature for reaction for 1-2h, cooling to room temperature, carrying out vacuum filtration, washing with deionized water until no bromide ion exists, drying a filter cake at 100 ℃, and finally grinding to 250 meshes to obtain modified bentonite for later use;
2) mixing: and (3) taking the component A and the component B, putting the component A and the component B into a stirrer, fully stirring for 1-2h, adding the component C, and fully stirring again to obtain a finished product.
Preferably, the modifier in step 1) is cetyltrimethylammonium bromide (solid).
Preferably, the mass ratio of the component A, the component B and the component C in the step 2) is 2-4:1:1, and the stirring time in the step 2) is 30-40 min.
(III) advantageous effects
Compared with the prior art, the invention provides the high thixotropic modified epoxy resin steel adhesive and the preparation method thereof, and the high thixotropic modified epoxy resin steel adhesive has the following beneficial effects:
according to the high thixotropic modified epoxy resin steel-sticking adhesive and the preparation method thereof, the tensile strength of a colloid can be greatly improved by modifying filler bentonite, the shear strength of the colloid can be greatly improved by doping nano-silica, although the tensile strength can be reduced, the influence of the bonding surface condition (smoothness) of a bonding surface on the bonding performance is great, the more smooth the bonding surface is, the better the bonding performance is, the modified bentonite and the nano-silica simultaneously act, and the high thixotropic modified epoxy resin steel-sticking adhesive is resistant to corrosion of acid and alkali media, high in curing speed at normal temperature, free of volatile matters, non-toxic and harmless; the adhesive has high bonding strength, good toughness and impact resistance, and can ensure that the colloidal body has good stability in tensile strength and bonding performance.
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 first embodiment is as follows:
the high thixotropic modified epoxy resin steel adhesive comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 80 parts of epoxy resin, 7 parts of liquid nitrile rubber, 4 parts of alkyl glycidyl ether, 80 parts of active light calcium carbonate, 30 parts of active filler and 10 parts of toughening agent; the component B comprises the following components in parts by mass: 10 parts of wetting agent, 5 parts of CTAB modified bentonite, 15 parts of talcum powder, 1 part of coupling agent, 15 parts of nano silicon dioxide and 1 part of curing agent (1).
The active filler is active silica powder, the polymer is polyacrylate, and the toughening agent is a mixture with different active end groups and different types of chain segments connected through ester bonds or urethane bonds.
In the embodiment, the wetting agent is sulfonated oil, the curing agent (1) is polyisocyanate, the component C is 25 parts of the curing agent (2), the curing agent (2) is low-molecular polyamide, the epoxy resin is bisphenol A diglycidyl ether, and the coupling agent is methacryloxypropyltrimethoxysilane which is an organic functional group silane coupling agent.
A preparation method of high thixotropic modified epoxy resin steel adhesive comprises the following steps:
1) preparation: weighing 8g of modifier, namely hexadecyl trimethyl ammonium bromide (solid), adding the modifier into a 1000mL beaker, then adding 792mL of deionized water, heating and stirring until the solid is dissolved, adding 80g of bentonite when the water temperature is constant at 84 ℃, stirring at constant temperature for reaction for 1h, cooling to room temperature, carrying out vacuum filtration, washing with deionized water until no bromide ion exists, drying a filter cake at 100 ℃, and finally grinding to 250 meshes to obtain modified bentonite for later use;
2) mixing: and (3) taking the component A and the component B, putting the component A and the component B into a stirrer, fully stirring for 1h, adding the component C, wherein the mass ratio of the component A to the component B to the component C is 2:1:1, fully stirring again to obtain a finished product, and stirring again for 30 min.
Example two:
the high thixotropic modified epoxy resin steel adhesive comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 90 parts of epoxy resin, 10 parts of liquid nitrile rubber, 7 parts of alkyl glycidyl ether, 115 parts of active light calcium carbonate, 35 parts of active filler and 12 parts of toughening agent; the component B comprises the following components in parts by mass: 15 parts of wetting agent, 7 parts of CTAB modified bentonite, 23 parts of talcum powder, 3 parts of coupling agent, 23 parts of nano silicon dioxide and 2 parts of curing agent (1).
The active filler is active silica powder, the polymer is polyacrylate, and the toughening agent is a mixture with different active end groups and different types of chain segments connected through ester bonds or urethane bonds.
In the embodiment, the wetting agent is sulfonated oil, the curing agent (1) is polyisocyanate, the component C is 28 parts of the curing agent (2), the curing agent (2) is low-molecular polyamide, the epoxy resin is bisphenol A diglycidyl ether, and the coupling agent is methacryloxypropyltrimethoxysilane which is an organic functional group silane coupling agent.
A preparation method of high thixotropic modified epoxy resin steel adhesive comprises the following steps:
1) preparation: weighing 9g of modifier, namely hexadecyl trimethyl ammonium bromide (solid), adding the modifier into a 1000mL beaker, then adding 792mL of deionized water, heating and stirring until the solid is dissolved, adding 80g of bentonite when the water temperature is constant at 84 ℃, stirring at constant temperature for reaction for 1h, cooling to room temperature, carrying out vacuum filtration, washing with deionized water until no bromide ion exists, drying a filter cake at 100 ℃, and finally grinding to 250 meshes to obtain modified bentonite for later use;
2) mixing: and (3) taking the component A and the component B, fully stirring the components in the stirrer for 1 hour, adding the component C, fully stirring the components A, B and C again to obtain a finished product, wherein the mass ratio of the component A to the component B to the component C is 3:1:1, and stirring the components again for 35 minutes.
Example three:
the high thixotropic modified epoxy resin steel adhesive comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 100 parts of epoxy resin, 14 parts of liquid nitrile rubber, 10 parts of alkyl glycidyl ether, 145 parts of active light calcium carbonate, 40 parts of active filler and 15 parts of toughening agent; the component B comprises the following components in parts by mass: 20 parts of wetting agent, 10 parts of CTAB modified bentonite, 30 parts of talcum powder, 5 parts of coupling agent, 30 parts of nano silicon dioxide and 3 parts of curing agent (1).
The active filler is active silica powder, the polymer is polyacrylate, and the toughening agent is a mixture with different active end groups and different types of chain segments connected through ester bonds or urethane bonds.
In the embodiment, the wetting agent is sulfonated oil, the curing agent (1) is polyisocyanate, the component C is 35 parts of the curing agent (2), the curing agent (2) is low-molecular polyamide, the epoxy resin is bisphenol A diglycidyl ether, and the coupling agent is methacryloxypropyltrimethoxysilane which is an organic functional group silane coupling agent.
A preparation method of high thixotropic modified epoxy resin steel adhesive comprises the following steps:
1) preparation: weighing 10g of modifier, namely hexadecyl trimethyl ammonium bromide (solid), adding the modifier into a 1000mL beaker, then adding 792mL of deionized water, heating and stirring until the solid is dissolved, adding 80g of bentonite when the water temperature is constant at 84 ℃, stirring at constant temperature for reaction for 2h, cooling to room temperature, carrying out vacuum filtration, washing with deionized water until no bromide ion exists, drying a filter cake at 100 ℃, and finally grinding to 250 meshes to obtain modified bentonite for later use;
2) mixing: and (3) taking the component A and the component B, fully stirring the components in the stirrer for 2 hours, adding the component C, fully stirring the components A, B and C again to obtain a finished product, wherein the mass ratio of the component A to the component B to the component C is 4:1:1, and stirring the components again for 40 min.
The invention has the beneficial effects that: the modified bentonite and the nano silica simultaneously act, because of active groups in the structure, the modified bentonite and the nano silica participate in the curing reaction of epoxy resin to form a part of a net structure finally formed by main resin, and the active silica powder does not have the defect of reduced adhesive force of an adhesive layer due to solvent volatilization, can effectively improve the adhesive force and hydrophobic interface performance of the epoxy resin and the silica powder, is reacted and crosslinked with a resin curing agent, thereby improving the mechanical strength, elastic modulus, shear strength and adhesive strength of a cured product, The thermal aging performance, the weather resistance and the like can ensure that the colloid has good stability in tensile strength and bonding performance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. The high thixotropic modified epoxy resin steel adhesive comprises a component A, a component B and a component C, and is characterized in that the component A comprises the following components in parts by mass: 80-100 parts of epoxy resin, 7-14 parts of liquid nitrile rubber, 4-10 parts of alkyl glycidyl ether, 80-145 parts of active light calcium carbonate, 30-40 parts of active filler and 10-15 parts of toughening agent; the component B comprises the following components in parts by mass: 10-20 parts of wetting agent, 5-10 parts of CTAB modified bentonite, 15-30 parts of talcum powder, 1-5 parts of coupling agent, 15-30 parts of nano silicon dioxide, 1-3 parts of curing agent (1) and 10-20 parts of polymer.
2. The high thixotropic modified epoxy resin steel adhesive according to claim 1, wherein the active filler is active silica powder, the polymer is polyacrylate, and the toughening agent is a mixture with different active end groups connecting different types of chain segments through ester bonds or urethane bonds.
3. The high thixotropic modified epoxy resin steel adhesive according to claim 1, wherein the wetting agent is sulfonated oil, the curing agent (1) is polyisocyanate, the component C is 25-35 parts of the curing agent (2), and the curing agent (2) is low molecular polyamide.
4. The high thixotropic modified epoxy resin steel adhesive according to claim 1, wherein the epoxy resin is bisphenol A diglycidyl ether, and the coupling agent is methacryloxypropyltrimethoxysilane, which is an organofunctional silane coupling agent.
5. A preparation method of high thixotropic modified epoxy resin steel adhesive is characterized by comprising the following steps:
1) preparation: weighing 8-10g of modifier, adding the modifier into a 1000mL beaker, adding 792mL of deionized water, heating and stirring until the solid is dissolved, adding 80g of bentonite when the water temperature is constant at 84 ℃, stirring at constant temperature for reaction for 1-2h, cooling to room temperature, carrying out vacuum filtration, washing with deionized water until no bromide ion exists, drying a filter cake at 100 ℃, and finally grinding to 250 meshes to obtain modified bentonite for later use;
2) mixing: and (3) taking the component A and the component B, putting the component A and the component B into a stirrer, fully stirring for 1-2h, adding the component C, and fully stirring again to obtain a finished product.
6. The method for preparing high thixotropic modified epoxy resin steel adhesive according to claim 5, wherein the temperature during heating and stirring in step 1) is 24-26 ℃, and the modifier in step 1) is cetyl trimethyl ammonium bromide (solid).
7. The preparation method of the high thixotropic modified epoxy resin steel adhesive according to claim 5, wherein the mass ratio of the component A, the component B and the component C in the step 2) is 2-4:1:1, and the re-stirring time in the step 2) is 30-40 min.
CN202210764921.XA 2022-07-01 2022-07-01 High-thixotropy modified epoxy resin steel adhesive and preparation method thereof Pending CN115029090A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678473A (en) * 2022-11-09 2023-02-03 宁夏中色新材料有限公司 Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678473A (en) * 2022-11-09 2023-02-03 宁夏中色新材料有限公司 Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof

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