CN113861905A - Easily-operated toughened epoxy composite adhesive and preparation method thereof - Google Patents
Easily-operated toughened epoxy composite adhesive and preparation method thereof Download PDFInfo
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- CN113861905A CN113861905A CN202110968803.6A CN202110968803A CN113861905A CN 113861905 A CN113861905 A CN 113861905A CN 202110968803 A CN202110968803 A CN 202110968803A CN 113861905 A CN113861905 A CN 113861905A
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to the technical field of epoxy adhesives, and provides an easy-to-operate toughened epoxy composite adhesive and a preparation method thereof, wherein the epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises the following components in parts by mass 1-2: 1, the component A is prepared from the following raw materials in parts by mass: 50-70 parts of epoxy resin, 30-50 parts of modified toughened epoxy resin, 1-5 parts of reactive diluent, 1-5 parts of coupling agent, 0-1 part of auxiliary agent, 10-30 parts of filler and 0.5-3 parts of thixotropic agent; the component B comprises the following raw materials in parts by mass: 60-90 parts of flexible curing agent, 10-40 parts of modified amine curing agent, 1-5 parts of coupling agent, 0-1 part of auxiliary agent, 0-10 parts of filler and 0.5-3 parts of thixotropic agent. The invention has high-strength adhesion and flexibility for the base material, and solves the problems of easy cracking, false adhesion and the like caused by the fact that the epoxy adhesive has rigidity and is not shock-resistant in the transportation process of epoxy adhesive composite adhesion.
Description
Technical Field
The invention relates to the technical field of epoxy adhesives, in particular to an easy-to-operate toughening type epoxy composite adhesive and a preparation method thereof.
Background
The excellent physical mechanical and electrical insulation properties of epoxy resins, their adhesion to various materials, and their flexibility in the process of use are not available with other thermosets. Therefore, the material can be made into coating, composite materials, casting materials, adhesives, mould pressing materials and injection molding materials, and is widely applied in various fields of national economy. Epoxy resins are not good in adhesion to nonpolar plastics such as polyolefin, and are used for various metal materials such as aluminum, iron, and copper; non-metallic materials such as glass, wood, concrete, etc.; thermosetting plastics such as phenolic aldehyde, amino, unsaturated polyester and the like have excellent bonding performance, so that the adhesive is called a universal adhesive. Epoxy adhesives are an important class of structural adhesives. The honeycomb composite board is an application of a common epoxy adhesive, the surface base material can be stone, metal, phenolic resin and the like, and the honeycomb composite board can be mainly used for lightening the same material (even the weight of the honeycomb composite board made of the base material with the same thickness is only 1/3 of the original compact base material) and reducing the price of the special material on the surface. Although most people meet the bonding strength during compounding, the epoxy adhesive is rigid in the transportation vibration or natural accelerated aging process, so that the adhesive layer is easy to crack, fall off and performance is easy to attenuate, and great potential safety hazards exist in the process.
Chinese patent CN107779147A discloses a high-strength epoxy honeycomb adhesive and a preparation method thereof, wherein the epoxy adhesive is a bi-component epoxy adhesive, when in use, a first component and a second component are mixed according to a weight ratio of 2-4:1, and the first component is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 5-10 parts of low-viscosity epoxy resin, 3-8 parts of active toughening agent, 10-20 parts of reinforcing filler, 10-20 parts of flame retardant and 0.3-3 parts of thixotropic agent, wherein the second component is prepared from the following raw materials in parts by weight: 50-90 parts of toughening curing agent, 10-20 parts of hardening curing agent and 0.3-1 part of coupling agent.
The main characteristic of the patent application is that the adhesive strength has small discreteness (high strength), and has rigidity and toughness, so that the main component in the formula adopts a curing system of polyfunctional group resin for improving the crosslinking density, and simultaneously adopts an active toughening agent and a toughening curing agent for improving the toughness. However, most of the polyfunctional groups have high viscosity, and the filler and the thixotropic agent are added, so that the whole viscosity thickening construction is not easy to operate, when the toughening curing agent is used as the crosslinking agent, the crosslinking density is reduced, and the bonding strength is influenced to a certain extent.
Disclosure of Invention
The invention aims to solve the problems that most of polyfunctional groups have high viscosity, a filler and a thixotropic agent are added, the whole viscosity thickening construction is not easy to operate, the crosslinking density is reduced and the bonding strength is influenced to a certain extent when a toughening curing agent is used as a crosslinking agent, and particularly, the functional toughening type is used, an elastomer (such as nitrile rubber) filled in the functional toughening type does not participate in the reaction, and the aging process is likely to migrate out of the surface to influence the bonding strength.
In order to achieve the purpose, the invention provides the following technical scheme: an easy-to-operate toughening epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises the following components in parts by mass 1-2: 1, carrying out proportioning composition to obtain the composition,
the component A comprises the following raw materials in parts by mass:
the component B comprises the following raw materials in parts by mass:
preferably, the epoxy resin comprises one or a mixture of more than two of bisphenol F epoxy resin, bisphenol A epoxy resin, phenolic aldehyde epoxy resin and polyfunctional epoxy resin.
Preferably, the toughening epoxy resin is one or a mixture of more than two of polyurethane modified epoxy resin, EPU modified epoxy resin, organosilicon modified epoxy resin and CTBN elastomer modified epoxy resin.
Preferably, the reactive diluent is one or a mixture of more than two of benzyl glycidyl ether, butyl glycidyl ether, C12-C14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether and 1, 6-hexanediol diglycidyl ether.
Preferably, the coupling agent is one or a mixture of more than two of gamma-glycidoxypropyltrimethoxysilane (KH-560), gamma-methacryloxypropyltrimethoxysilane (KH-570), vinyltrimethoxysilane and vinyltris (beta-methoxyethoxy) silane.
Preferably, the auxiliary agent is one or a mixture of more than two of modified urea solution (BYK-410), tributyl phosphate, acidic polyester solution (BYK-985), a foam breaking polymer, polysiloxane solution (BYK-A530), foam breaking polysiloxane, high molecular weight block copolymer solution (BYK-110) and polyether modified polydimethylsiloxane copolymer (BYK-333).
Preferably, the filler is one or a mixture of more than two of silica powder, white corundum, aluminum hydroxide, titanium white powder, silicon carbide, calcium carbonate and carbon black with 325 meshes, 500 meshes, 800 meshes, 1000 meshes, 1250 meshes, 2000 meshes, 3000 meshes, 5000 meshes, 8000 meshes and 10000 meshes.
Preferably, the flexible curing agent is one or a mixture of two or more of polyether amine, polyamide and polyimide.
Preferably, the amine curing agent is one or a mixture of more than two of aromatic polyamine and modified aromatic amine, alicyclic polyamine and modified alicyclic amine, phenolic polyamine and modified phenolic amine; the thixotropic agent is one or a mixture of more than two of gas phase white carbon black LM-150, organic bentonite, precipitated silica SQ-180, nano silicon dioxide and nano montmorillonite.
Preferably, the preparation method of the easy-to-operate toughened epoxy composite adhesive comprises the following process steps:
1) preparation of component A: adding epoxy resin, toughening epoxy resin, reactive diluent, coupling agent and auxiliary agent into a power mixer, stirring at normal temperature for 60 minutes, uniformly mixing, adding filler, continuously stirring for 120 minutes, adding thixotropic agent, continuously stirring for 30 minutes, vacuumizing and stirring for 10 minutes to obtain a component A for later use;
2) preparation of the component B: adding a polythiol curing agent, a modified amine curing agent, an accelerator and an auxiliary agent into a reaction kettle, stirring at normal temperature for 60 minutes, uniformly mixing, then adding a filler, continuing to stir for 120 minutes, then adding a thixotropic agent, continuing to stir for 30 minutes, and vacuumizing and stirring for 10 minutes to obtain a component B for later use;
3) mixing and stirring: mixing the component A and the component B according to the weight ratio of 1-2: 1, uniformly mixing to obtain an easy-to-operate toughened epoxy composite adhesive finished product for use.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts the normal temperature curing two-component epoxy glue for bonding, and has the advantages of excellent bonding strength, high thixotropy, aging resistance, simple and convenient operation, vibration resistance and the like on various materials (except plastic PP/ABS/PC and the like). The epoxy composite adhesive is easy to operate and toughened. The easy-to-operate toughened epoxy composite adhesive has the advantages of low volatility, low toxicity, curing time adjustability, good weather resistance, high hardness, good flexibility, hand comfort during operation of main workers and good bonding effect during aging resistance, and is favorable for popularization.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following 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.
One specific application of this embodiment is:
example 1:
the preferable easy-to-operate toughening epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises the following components in parts by mass 1:1, carrying out proportioning composition to obtain the composition,
the component A comprises the following components: NPEL-12870 kg, polyurethane modified epoxy resin 30kg, benzyl glycidyl ether 2.5kg, KH-5601.2 kg, BYK-3330.5 kg, 1250-mesh silica powder 10kg, and gas phase white carbon black LM-1501 kg.
The preparation process of the component A comprises the following steps: adding NPEL 128, polyurethane modified epoxy resin, benzyl glycidyl ether, BYK-333 and KH-560 into a power mixer, stirring for 60 minutes at normal temperature, adding 1250-mesh silicon powder, continuously stirring for 120 minutes, adding fumed silica LM-150, continuously stirring for 30 minutes, vacuumizing, stirring for 10 minutes, and uniformly mixing for later use;
the component B comprises the following components: 80kg of polyamide, 10kg of modified alicyclic amine, BYK-3330.3 kg, KH-5501.5 kg and 3kg of fumed silica
The preparation process of the component B comprises the following steps: adding polyamide, modified alicyclic amine, BYK-333 and KH-560 into a reaction kettle, stirring at normal temperature for 60 minutes, adding fumed silica, continuing stirring for 30 minutes, vacuumizing and stirring for 10 minutes, and uniformly mixing for later use;
and (3) performance testing: and (3) mixing the prepared component A and the component B according to the ratio of A: mixing B-1: 1, stirring uniformly, standing and curing for 24h, wherein the operation time is 60 min, the curing time is 4h and 30 min, the hardness is 75D, the aluminum sheet shear strength is 3003 at 25 ℃ and 15MPa, the roller peeling force is 130 N.mm/mm, and the mixed glue solution has high thixotropy.
Example 2:
the preferable easy-to-operate toughening epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises the following components in parts by mass: 1, carrying out proportioning composition to obtain the composition,
the component A comprises the following components: : AFG-9030 kg, NPEL-12830 kg, polyurethane modified epoxy resin 20kg, organic silicon modified epoxy resin 5kg, AGE 5kg, KH-5602 kg, BYK-A5300.67kg, nano calcium carbonate 15kg, organic bentonite 1kg and fumed silica LM-1501 kg.
The preparation process comprises the following steps: adding AFG-90, NPEL-128, polyurethane modified epoxy resin, organic silicon modified epoxy resin, AGE, BYK-A530 and KH-560 into a power mixer, stirring for 60 minutes at normal temperature, adding nano calcium carbonate and organic bentonite, continuously stirring for 120 minutes, adding fumed silica LM-150, continuously stirring for 30 minutes, vacuumizing and stirring for 10 minutes, and uniformly mixing for later use;
the component B comprises the following components: 70kg of polyether amine curing agent, 15kg of modified fatty amine, BYK-A5300.67kg, KH-5702 kg, 5kg of nano calcium carbonate, 0.5kg of organic bentonite and SQ-1802 kg of precipitated white carbon black
The preparation process comprises the following steps: adding a polyether amine curing agent, modified fatty amine, BYK-A530 and KH-570 into a reaction kettle, stirring for 60 minutes at normal temperature, adding nano calcium carbonate and organic bentonite, continuing stirring for 120 minutes, adding precipitated white carbon black SQ-180, continuing stirring for 30 minutes, vacuumizing, stirring for 10 minutes, and uniformly mixing for later use;
and (3) performance testing: and (3) mixing the prepared component A and the component B according to the ratio of A: mixing and stirring uniformly B-2: 1, standing and curing for 24h, wherein the operation time is 75 minutes, the curing time is 3 hours, the hardness is 76D, the shearing strength of 3003 aluminum sheets is 21MPa at 25 ℃, the roller peeling force is 150 N.mm/mm, and the mixed glue solution has high thixotropy.
Example 3:
the preferable easy-to-operate toughening epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises the following components in parts by mass: 1, carrying out proportioning composition to obtain the composition,
the component A comprises the following components: 63135 kg of NPEL, 12830 kg of NPEL, 20kg of EPU modified epoxy resin, 20kg of CTBN modified epoxy resin, 4.6kg of 1, 6-hexanediol diglycidyl ether, 4.7kg of vinyl trimethoxy silane, BYK-A5300.70kg, 20kg of 600 mesh aluminum hydroxide and 3kg of nano silicon dioxide
The preparation process of the component A comprises the following steps: adding NPEL 631, NPEL 128, EPU modified epoxy resin, CTBN modified epoxy resin, 1, 6-hexanediol diglycidyl ether, vinyl trimethoxy silane and BYK-A530 into a power mixer, stirring at normal temperature for 60 minutes, adding 600-mesh aluminum hydroxide, continuously stirring for 120 minutes, adding nano silicon dioxide, continuously stirring for 30 minutes, vacuumizing and stirring for 10 minutes, and uniformly mixing for later use;
the component B comprises the following components: 30kg of polyamide curing agent, 32kg of polyether amine curing agent, 36kg of modified fatty amine curing agent, BYK-A5300.71kg, 3kg of vinyl trimethoxy silane, 8kg of 600-mesh aluminum hydroxide, 2kg of white corundum and 1kg of nano silicon dioxide
The preparation process of the component B comprises the following steps: adding a polyamide curing agent, a polyether amine curing agent, a modified fatty amine curing agent, BYK-A530 and vinyl trimethoxy silane into a reaction kettle, stirring for 60 minutes at normal temperature, adding 600-mesh aluminum hydroxide and white corundum, continuously stirring for 120 minutes, adding nano silicon dioxide, continuously stirring for 30 minutes, vacuumizing and stirring for 10 minutes, and uniformly mixing for later use;
and (3) performance testing: and (3) mixing the prepared component A and the component B according to the ratio of A: mixing B with the ratio of 2:1, stirring uniformly, standing and curing for 24h, wherein the operation time is 67 minutes, the curing time is 3.7 hours, the hardness is 75D, the shearing strength of 3003 aluminum sheets is 19MPa after being ground at 25 ℃, the roller stripping force is 125 N.mm/mm, and the mixed glue solution has high thixotropy.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, a schematic representation of the above terms does not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. An easy-to-operate toughening epoxy composite adhesive comprises a component A and a component B, wherein the component A comprises, by mass, 1-2: 1, the formula is characterized in that:
the component A comprises the following raw materials in parts by mass:
the component B comprises the following raw materials in parts by mass:
2. the easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the epoxy resin comprises one or a mixture of more than two of bisphenol F epoxy resin, bisphenol A epoxy resin, novolac epoxy resin and polyfunctional epoxy resin.
3. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the toughening epoxy resin is one or a mixture of more than two of polyurethane modified epoxy resin, EPU modified epoxy resin, organic silicon modified epoxy resin and CTBN elastomer modified epoxy resin.
4. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the active diluent is one or a mixture of more than two of benzyl glycidyl ether, butyl glycidyl ether, C12-C14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether and 1, 6-hexanediol diglycidyl ether.
5. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the coupling agent is one or a mixture of more than two of gamma-glycidoxypropyltrimethoxysilane (KH-560), gamma-methacryloxypropyltrimethoxysilane (KH-570), vinyl trimethoxysilane and vinyl tri (beta-methoxyethoxy) silane.
6. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the auxiliary agent is one or a mixture of more than two of modified urea solution (BYK-410), tributyl phosphate, acidic polyester solution (BYK-985), a foam breaking polymer, polysiloxane solution (BYK-A530), foam breaking polysiloxane, high molecular weight block copolymer solution (BYK-110) and polyether modified polydimethylsiloxane copolymer (BYK-333).
7. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the filler is one or a mixture of more than two of silica powder, white corundum, aluminum hydroxide, titanium dioxide, silicon carbide, calcium carbonate and carbon black with 325 meshes, 500 meshes, 800 meshes, 1000 meshes, 1250 meshes, 2000 meshes, 3000 meshes, 5000 meshes, 8000 meshes and 10000 meshes.
8. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the flexible curing agent is one or a mixture of more than two of polyether amine, polyamide and polyimide.
9. The easy-to-handle toughened epoxy composite adhesive according to claim 1, wherein: the amine curing agent is one or a mixture of more than two of aromatic polyamine and modified aromatic amine, alicyclic polyamine and modified alicyclic amine, phenolic polyamine and modified phenolic amine; the thixotropic agent is one or a mixture of more than two of gas phase white carbon black LM-150, organic bentonite, precipitated silica SQ-180, nano silicon dioxide and nano montmorillonite.
10. The preparation method of the easy-to-operate toughening epoxy composite adhesive according to claims 1 to 9, characterized in that: the method comprises the following process steps:
1) preparation of component A: adding epoxy resin, toughening epoxy resin, reactive diluent, coupling agent and auxiliary agent into a power mixer, stirring at normal temperature for 60 minutes, uniformly mixing, adding filler, continuously stirring for 120 minutes, adding thixotropic agent, continuously stirring for 30 minutes, vacuumizing and stirring for 10 minutes to obtain a component A for later use;
2) preparation of the component B: adding a polythiol curing agent, a modified amine curing agent, an accelerator and an auxiliary agent into a reaction kettle, stirring at normal temperature for 60 minutes, uniformly mixing, then adding a filler, continuing to stir for 120 minutes, then adding a thixotropic agent, continuing to stir for 30 minutes, and vacuumizing and stirring for 10 minutes to obtain a component B for later use;
3) mixing and stirring: mixing the component A and the component B according to the weight ratio of 1-2: 1, uniformly mixing to obtain an easy-to-operate toughened epoxy composite adhesive finished product for use.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369436A (en) * | 2022-01-17 | 2022-04-19 | 湛江港石化码头有限责任公司 | Nano modified anti-leakage constant-fire repairing elastic material |
| CN114686152A (en) * | 2022-04-24 | 2022-07-01 | 中国电建集团中南勘测设计研究院有限公司 | Perfusion/pressure-injection type epoxy resin structural adhesive and application thereof |
| CN115074068A (en) * | 2022-07-22 | 2022-09-20 | 北京高盟新材料股份有限公司 | Double-component epoxy adhesive and preparation method thereof |
-
2021
- 2021-08-23 CN CN202110968803.6A patent/CN113861905A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369436A (en) * | 2022-01-17 | 2022-04-19 | 湛江港石化码头有限责任公司 | Nano modified anti-leakage constant-fire repairing elastic material |
| CN114686152A (en) * | 2022-04-24 | 2022-07-01 | 中国电建集团中南勘测设计研究院有限公司 | Perfusion/pressure-injection type epoxy resin structural adhesive and application thereof |
| CN114686152B (en) * | 2022-04-24 | 2023-10-27 | 中国电建集团中南勘测设计研究院有限公司 | Pouring/pressure-pouring type epoxy resin structural adhesive and application thereof |
| CN115074068A (en) * | 2022-07-22 | 2022-09-20 | 北京高盟新材料股份有限公司 | Double-component epoxy adhesive and preparation method thereof |
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