CN110982464A - Toughening epoxy adhesive capable of being reprocessed and recycled and curing method - Google Patents
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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
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
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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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Abstract
The application relates to a toughening epoxy adhesive capable of being reprocessed and recycled and a curing method, wherein the toughening epoxy adhesive capable of being reprocessed and recycled comprises the following raw materials in parts by mass: 100 parts of epoxy resin, 15-35 parts of curing agent diamino diphenyl disulfide and 20-70 parts of flexibilizer aromatic amine terminated polysulfide resin, wherein the flexibilizer aromatic amine terminated polysulfide resin comprises the following raw materials in parts by mass: 100 parts of mercapto-terminated liquid polysulfide resin, 6-25 parts of diamino diphenyl disulfide, 0.1 part of tertiary amine, 5 parts of hydrogen peroxide and 150 parts of solvent-selected methane dioxide; the curing agent and the toughening agent both contain the same reversible covalent bond, so that the dynamic reversibility of the whole cross-linked structure is realized, network rearrangement is initiated to ensure that the epoxy adhesive has reworkability and recoverability, the retention rate of the main performance exceeds 90 percent after three times of circulation, and the problems of environmental pollution and resource waste caused by waste high polymer materials can be effectively solved.
Description
Technical Field
The invention belongs to the technical field of epoxy adhesives, and particularly relates to a toughening epoxy adhesive capable of being reprocessed and recycled and a curing method.
Background
As a typical thermosetting material, the epoxy adhesive has excellent tensile strength, wear resistance, medium resistance, electrical insulation performance and bonding performance, and is widely applied to the fields of aerospace, ships, electronics, machinery and the like. The epoxy adhesive without toughening modification has the problems of large brittleness, low elongation at break, poor impact resistance and the like, and the application range of the epoxy adhesive is limited, so the epoxy adhesive is generally used after toughening modification.
At present, the toughened epoxy adhesive commonly used at home and abroad is usually obtained by curing components such as epoxy resin, a curing agent, a toughening agent and the like, and molecular structures of the components are bonded in a non-reversible covalent bond mode to show the typical characteristics of a thermosetting material. However, the thermosetting materials can not meet the requirements of the current society on material recycling, environmental protection and the like. In recent years, the epoxy resin is crosslinked by reversible dynamic bonds to realize the reprocessing recycling of the materials, for example, patent CN201611093870.3 discloses a recyclable epoxy resin and a curing method, wherein a polyamine curing agent with a dynamic imine bridging bond structure is synthesized, and the epoxy resin is crosslinked and cured to obtain the epoxy resin with recycling performance. At present, all the reported recyclable epoxy resins are non-toughened systems, and although the recycling property is realized, the problems of large brittleness, low elongation at break, poor impact resistance and the like exist in the body.
In the toughened epoxy adhesive, the components of a crosslinked epoxy resin network are jointly completed by a curing agent and a toughening agent, and the key for realizing the reutilization is that the whole crosslinked structure contains reversible dynamic chemical bonds, so that the network rearrangement is initiated to realize the reutilization. Therefore, on the basis of ensuring the toughness of the epoxy adhesive, reversible dynamic crosslinking between two components of the curing agent and the toughening agent is realized, the epoxy adhesive which has high toughness and reprocessing and recycling performance is obtained, and the focus of industrial attention is formed.
Disclosure of Invention
The technical problem to be solved is as follows: the application mainly provides a toughening epoxy adhesive capable of being reprocessed and recycled and a curing method, solves the technical problems that the toughening and the reprocessing recycling performances of the existing epoxy adhesive cannot be compatible in the prior art, provides an epoxy adhesive with high toughness and reprocessing recycling performances, and explains the curing method.
The technical scheme is as follows:
the toughening epoxy adhesive capable of being reprocessed and recycled comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 15-35 parts of curing agent diamino diphenyl disulfide and 20-70 parts of flexibilizer aromatic amino terminated polysulfide resin.
As a preferred technical scheme of the invention: the toughening agent aromatic amine terminated polysulfide resin comprises the following raw materials in parts by mass: 100 parts of mercapto-terminated liquid polysulfide resin, 6-25 parts of diamino diphenyl disulfide, 0.1 part of tertiary amine, 5 parts of hydrogen peroxide and 150 parts of solvent-selected methane dioxide.
As a preferred technical scheme of the invention: the epoxy resin is one or two of bisphenol A type epoxy resin and bisphenol F type epoxy resin.
As a preferred technical scheme of the invention: the curing agent diaminodiphenyl disulfide is one or two of 2, 2 '-diaminodiphenyl disulfide and 4, 4' -diaminodiphenyl disulfide.
As a preferred technical scheme of the invention: the molecular weight of the end-thinning liquid polysulfide resin is 1000-4000.
As a preferred technical scheme of the invention: the tertiary amine is one or a combination of triethylamine, triethanolamine and 2, 4, 6-tris (dimethylaminomethyl) phenol.
As a preferred technical scheme of the invention: the reprocessing recycling method comprises the steps of carrying out hot pressing on the crushed toughened epoxy adhesive for 30 minutes at the temperature of 150 ℃ and under the pressure of 12MPa to reform the complete toughened epoxy adhesive, and circulating for three times, wherein the tensile strength, the elongation at break and the impact strength are compared with the retention rate of the initial epoxy adhesive, namely the sample performance data/the initial sample performance data after hot pressing exceed 90%.
The invention also discloses a curing method of the toughening epoxy adhesive capable of being reprocessed and recycled, which comprises the following steps:
the first step is as follows: weighing 100 parts of sulfhydryl-terminated liquid polysulfide resin, 6-25 parts of diaminodiphenyl disulfide, 0.1 part of tertiary amine, 5 parts of hydrogen peroxide and 150 parts of solvent-selected methane dioxide according to the mass part ratio;
the second step is that: adding a sulfydryl-terminated liquid polysulfide resin, diaminodiphenyl disulfide, tertiary amine and a solvent, namely methane dioxide, into a reaction bottle under the protection of nitrogen, stirring, refluxing and heating to 120-150 ℃, reacting for 18-36 hours to ensure that disulfide bonds in diaminodiphenyl disulfide and disulfide bonds in a polysulfide resin main chain are fully exchanged, monitoring the reaction process by adopting thin-layer chromatography (TLC) until the raw material points of diaminodiphenyl disulfide completely disappear, cooling to 60 ℃, adding hydrogen peroxide, reacting for 12 hours under the protection of nitrogen to ensure that sulfydryl is completely oxidized and coupled, monitoring the sulfydryl by adopting infrared spectroscopy (2562 cm)-1Has an absorption peak at the endCompletely disappearing, cooling to obtain the flexibilizer aromatic amino terminated polysulfide resin;
the third step: weighing 100 parts of epoxy resin, 15-35 parts of curing agent diaminodiphenyl disulfide and 20-70 parts of flexibilizer aromatic amino terminated polysulfide resin according to the mass parts;
the fourth step: uniformly mixing epoxy resin, a curing agent diaminodiphenyl disulfide and a toughening agent aromatic amino terminated polysulfide resin;
the fifth step: centrifuging and defoaming the mixture, pouring the mixture into a mold, and naturally leveling;
and a sixth step: curing at 60 ℃ for 3 days or curing at 70 ℃ for 2 days to obtain the toughening epoxy adhesive which can be reprocessed and recycled.
As a preferred technical scheme of the invention: the mixing method in the fourth step is mechanical stirring dispersion, the stirring speed is 100-.
As a preferred technical scheme of the invention: the fifth step of centrifugal defoaming adopts a planetary gravity centrifugal defoaming machine, the revolution speed is 2000-3000r/min, the rotation speed is 1400-2100r/min, the time is 2-5min, and the temperature is room temperature.
Has the advantages that: compared with the prior art, the toughening epoxy adhesive capable of being reprocessed and recycled and the curing method have the following technical effects:
1. the curing agent and the toughening agent both contain reversible dynamic disulfide bonds, and dynamic disulfide bond exchange can occur between the curing agent and the curing agent, between the toughening agent and the toughening agent, and between the curing agent and the toughening agent, which is the key for realizing repair and rearrangement of the whole cross-linked network of the material after fracture and the key for realizing reprocessing and recycling of the epoxy adhesive.
2. The curing agent and the toughening agent both contain aromatic amino structures, the compatibility of the curing agent and the toughening agent is high, the dynamic exchange of disulfide bonds is facilitated, the reactive groups both have a plurality of reactive sites, the reactive groups react with epoxy resin to form a stable crosslinking structure, and the aromatic base structure and the rigid structure can ensure the mechanical strength of the material.
3. The main chain of the toughening agent is of a polysulfide structure, the flexibility at low temperature is good, the toughening agent has good compatibility with epoxy resin, the epoxy adhesive can be effectively toughened, a synergistic effect is generated between the epoxy adhesive and the epoxy adhesive, and the toughening effect of the epoxy adhesive is ensured.
4. The epoxy adhesive disclosed by the invention contains the same reversible covalent bond (disulfide bond) based on the curing agent and the toughening agent, so that the dynamic reversibility of the whole crosslinking structure is realized, the epoxy adhesive can be better recovered under the air hot-pressing condition, and no additive is required to be added during recovery, so that the toughening epoxy adhesive capable of being recycled is disclosed.
5. The epoxy adhesive has good elongation at break and impact strength by effectively toughening the epoxy resin through a flexible structure of polysulfide resin in the toughening agent, and the tensile strength, elongation at break and impact strength of the epoxy adhesive can be effectively adjusted by changing the using amounts of the curing agent and the toughening agent and the proportion of the polysulfide resin and the diaminodiphenyl disulfide in the toughening agent, so that the epoxy adhesives with different properties have good reworkability and recoverability. The tensile strength of the epoxy adhesive is 27.3 MPa-45.8 MPa, and the toughness is reflected by the following components: elongation at break of 5.6-22.8% and impact strength of 22.7kJ/m2～85.1kJ/m2The reworkable recycling performance is shown as follows: the crushed sample is hot pressed for 30 minutes at 150 ℃ and 12MPa, a complete sample can be formed again, and after three times of circulation, the retention rate of the tensile strength, the elongation at break and the impact strength are compared with the retention rate of the initial epoxy adhesive, namely the performance data of the sample/the performance data of the initial sample after hot pressing exceed 90 percent.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A method for curing a toughening epoxy adhesive capable of being reprocessed and recycled comprises the following steps:
the first step is as follows: preparing a toughening agent aromatic amine terminated polysulfide resin: weighing 100g of thiol-terminated liquid polysulfide resin with the relative molecular mass of 4000, 6.2g of 2, 2' -diaminodiphenyl disulfide, 0.1g of 2, 4, 6-tris (dimethylaminomethyl) phenol and 150g of solvent methylene dioxide, adding the weighed materials into a reaction flask, stirring, refluxing and heating at 120 ℃ under the protection of nitrogen, reacting for 24 hours to ensure that disulfide bonds in diaminodiphenyl disulfide and disulfide bonds in a polysulfide resin main chain are fully exchanged, monitoring the reaction process by adopting thin-layer chromatography (TLC) until the diaminodiphenyl disulfide raw material points completely disappear, cooling to 60 ℃, adding 5g of hydrogen peroxide, reacting for 12 hours under the protection of nitrogen, completely oxidatively coupling sulfhydryl, monitoring sulfhydryl by adopting infrared spectroscopy, wherein the sulfhydryl is 2562cm-1The absorption peak completely disappears, and the aromatic amine terminated polysulfide resin as the toughening agent is obtained after cooling;
the second step is that: the preparation of the toughening epoxy adhesive which can be reprocessed and recycled comprises the following steps: weighing 100g of bisphenol A type epoxy resin, 31.4g of curing agent 2, 2' -diaminodiphenyl disulfide and 20g of toughening agent aromatic amine terminated polysulfide resin, uniformly mixing the components, stirring at a speed of 100r/min for 8min at room temperature, centrifuging and defoaming, revolving at a speed of 2500r/min, rotating at a speed of 1750r/min for 3min at room temperature, pouring into a mold, naturally leveling, and curing at 60 ℃ for 3 days to obtain the toughening epoxy adhesive capable of being reprocessed and recycled.
Example 2
A method for curing a toughening epoxy adhesive capable of being reprocessed and recycled comprises the following steps:
the first step is as follows: preparing a toughening agent aromatic amine terminated polysulfide resin: weighing 100g of thiol-terminated liquid polysulfide resin with the relative molecular mass of 1000, 24.8g of 2, 2' -diaminodiphenyl disulfide, 0.1g of triethylamine and 150g of solvent methylene dioxide, adding the weighed materials into a reaction bottle, stirring, refluxing and heating the materials at 150 ℃ under the protection of nitrogen, reacting the materials for 36 hours to ensure that disulfide bonds in diaminodiphenyl disulfide and disulfide bonds in a polysulfide resin main chain are fully exchanged, monitoring the reaction progress by adopting thin-layer chromatography (TLC) until the raw material points of diaminodiphenyl disulfide completely disappear, cooling the reaction solution to 60 ℃, adding 5g of hydrogen peroxide, and reacting the mixture for 12 hours under the protection of nitrogen to ensure that thiol is fully oxidized and coupledMonitoring of sulfydryl of 2562cm by infrared spectroscopy-1The absorption peak completely disappears, and the aromatic amine terminated polysulfide resin as the toughening agent is obtained after cooling;
the second step is that: the preparation of the toughening epoxy adhesive which can be reprocessed and recycled comprises the following steps: weighing 100g of bisphenol A type epoxy resin, 18.7g of curing agent 4, 4' -diaminodiphenyl disulfide and 70g of toughening agent aromatic amine terminated polysulfide resin, uniformly mixing the components, stirring at the speed of 150r/min for 6min at room temperature, centrifuging and defoaming, revolving at the speed of 2000r/min, rotating at the speed of 1400r/min for 5min at room temperature, pouring into a mold, naturally leveling, and curing at 70 ℃ for 2 days to obtain the toughening epoxy adhesive capable of being reprocessed and recycled.
Example 3
A method for curing a toughening epoxy adhesive capable of being reprocessed and recycled comprises the following steps:
the first step is as follows: preparing a toughening agent aromatic amine terminated polysulfide resin: weighing 100g of thiol-terminated liquid polysulfide resin with the relative molecular mass of 4000, 6.2g of 4, 4' -diaminodiphenyl disulfide, 0.1g of triethanolamine and 150g of solvent methane dioxide, adding the weighed materials into a reaction bottle, stirring, refluxing and heating the materials at 130 ℃ under the protection of nitrogen, reacting the materials for 20 hours to ensure that disulfide bonds in diaminodiphenyl disulfide and disulfide bonds in a polysulfide resin main chain are fully exchanged, monitoring the reaction process by adopting thin-layer chromatography (TLC) until the diamino diphenyl disulfide raw material points completely disappear, cooling the reaction product to 60 ℃, adding 5g of hydrogen peroxide, reacting the reaction product for 12 hours under the protection of nitrogen to ensure that thiol is fully oxidatively coupled, monitoring thiol by adopting infrared spectroscopy, and ensuring that the-1The absorption peak completely disappears, and the aromatic amine terminated polysulfide resin as the toughening agent is obtained after cooling;
the second step is that: the preparation of the toughening epoxy adhesive which can be reprocessed and recycled comprises the following steps: weighing 100g of bisphenol F type epoxy resin, 34.2g of curing agent 2, 2' -diaminodiphenyl disulfide and 40g of toughening agent aromatic amine terminated polysulfide resin, uniformly mixing the components, stirring at the speed of 200r/min for 5min at room temperature, centrifuging and defoaming, revolving at the speed of 3000r/min, rotating at the speed of 2100r/min for 2min at room temperature, pouring into a mold, naturally leveling, and curing at 60 ℃ for 3 days to obtain the toughening epoxy adhesive capable of being reprocessed and recycled.
Example 4
A method for curing a toughening epoxy adhesive capable of being reprocessed and recycled comprises the following steps:
the first step is as follows: preparing a toughening agent aromatic amine terminated polysulfide resin: weighing 100g of terminal sulfydryl liquid polysulfide resin with the relative molecular mass of 2500, 9.9g of 2, 2' -diaminodiphenyl disulfide, 0.1g of triethanolamine and 150g of solvent methane dioxide, adding the weighed materials into a reaction bottle, stirring, refluxing and heating the materials at 140 ℃ under the protection of nitrogen, reacting the materials for 28 hours to ensure that disulfide bonds in diaminodiphenyl disulfide and disulfide bonds in a polysulfide resin main chain are fully exchanged, monitoring the reaction process by adopting thin-layer chromatography (TLC) until the raw material points of diaminodiphenyl disulfide completely disappear, cooling the reaction product to 60 ℃, adding 5g of hydrogen peroxide, reacting the mixture for 12 hours under the protection of nitrogen to ensure that sulfydryl is fully oxidatively coupled, monitoring the sulfydryl by adopting infrared-1The absorption peak completely disappears, and the aromatic amine terminated polysulfide resin as the toughening agent is obtained after cooling;
the second step is that: the preparation of the toughening epoxy adhesive which can be reprocessed and recycled comprises the following steps: weighing 50g of bisphenol A type epoxy resin, 50g of bisphenol F type epoxy resin, 10.1g of curing agent 2, 2 '-diaminodiphenyl disulfide, 19g of curing agent 4, 4' -diaminodiphenyl disulfide and 60g of toughening agent aromatic amine terminated polysulfide resin, uniformly mixing the components, stirring at the speed of 150r/min, stirring for 6min, temperature of room temperature, centrifugal defoaming, revolution speed of 2500r/min, rotation speed of 1750r/min, time of 3min, temperature of room temperature, pouring into a mold, natural leveling, and curing at 70 ℃ for 2 days to obtain the toughening epoxy adhesive capable of being reprocessed and recycled.
The performance of the epoxy adhesive was measured and the results are shown in table 1. Wherein, the reworkability recovery test is to test the performance of the sample obtained by hot pressing for 30 minutes under the conditions of 150 ℃ and 12MPa after the sample is crushed, the process is circulated for three times, and the performance data after the third circulation is recorded in the table.
TABLE 1 epoxy Adhesives and Main Properties after reprocessing
The above examples only illustrate some of the raw material ratios in this patent, and they are not illustrated herein. Modifications and substitutions to methods, steps or conditions of the present application are intended to be within the scope of the present application without departing from the spirit and substance of the present application.
Claims (10)
1. The toughening epoxy adhesive capable of being reprocessed and recycled is characterized by comprising the following components in parts by weight: the toughening epoxy adhesive capable of being reprocessed and recycled comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 15-35 parts of curing agent diamino diphenyl disulfide and 20-70 parts of flexibilizer aromatic amino terminated polysulfide resin.
2. The reworkable, recyclable toughened epoxy adhesive according to claim 1, wherein: the toughening agent aromatic amine terminated polysulfide resin comprises the following raw materials in parts by mass: 100 parts of mercapto-terminated liquid polysulfide resin, 6-25 parts of diamino diphenyl disulfide, 0.1 part of tertiary amine, 5 parts of hydrogen peroxide and 150 parts of dichloromethane serving as a solvent.
3. The reworkable, recyclable toughened epoxy adhesive according to claim 1, wherein: the epoxy resin is one or two of bisphenol A type epoxy resin and bisphenol F type epoxy resin.
4. The reworkable, recyclable toughened epoxy adhesive according to claim 1, wherein: the curing agent diaminodiphenyl disulfide is one or two of 2, 2 '-diaminodiphenyl disulfide and 4, 4' -diaminodiphenyl disulfide.
5. The reworkable, recyclable toughened epoxy adhesive according to claim 2, wherein: the molecular weight of the end-thinning liquid polysulfide resin is 1000-4000.
6. The reworkable, recyclable toughened epoxy adhesive according to claim 2, wherein: the tertiary amine is one or a combination of triethylamine, triethanolamine and 2, 4, 6-tris (dimethylaminomethyl) phenol.
7. The reworkable, recyclable toughened epoxy adhesive according to claim 1, wherein: the reprocessing recycling method comprises the steps of carrying out hot pressing on the crushed toughened epoxy adhesive for 30 minutes at the temperature of 150 ℃ and under the pressure of 12MPa to reform the complete toughened epoxy adhesive, and circulating for three times, wherein the tensile strength, the elongation at break and the impact strength are compared with the retention rate of the initial epoxy adhesive, namely the sample performance data/the initial sample performance data after hot pressing exceed 90%.
8. A method of curing a reworkable recyclable toughened epoxy adhesive according to any one of claims 1 to 7 comprising the steps of:
the first step is as follows: weighing 100 parts of sulfhydryl-terminated liquid polysulfide resin, 6-25 parts of diaminodiphenyl disulfide, 0.1 part of tertiary amine, 5 parts of hydrogen peroxide and 150 parts of dichloromethane serving as a solvent according to the mass part ratio;
the second step is that: adding a thiol-terminated liquid polysulfide resin, diaminodiphenyl disulfide, tertiary amine and a solvent dichloromethane into a reaction bottle under the protection of nitrogen, stirring, refluxing, heating to 120-150 ℃, reacting for 18-36 hours, fully exchanging disulfide bonds in diaminodiphenyl disulfide with disulfide bonds in a polysulfide resin main chain, monitoring the reaction process by adopting thin-layer chromatography TLC until the diaminodiphenyl disulfide raw material point completely disappears, cooling to 60 ℃, adding hydrogen peroxide, reacting for 12 hours under the protection of nitrogen, completely oxidatively coupling sulfhydryl, monitoring the complete disappearance of an absorption peak at 2562cm < -1 > of sulfhydryl by adopting an infrared spectroscopy, and cooling to obtain a flexibilizer aromatic amino group blocked polysulfide resin;
the third step: weighing 100 parts of epoxy resin, 15-35 parts of curing agent diaminodiphenyl disulfide and 20-70 parts of flexibilizer aromatic amino terminated polysulfide resin according to the mass part ratio;
the fourth step: uniformly mixing epoxy resin, a curing agent diaminodiphenyl disulfide and a toughening agent aromatic amino terminated polysulfide resin;
the fifth step: centrifuging and defoaming the mixture, pouring the mixture into a mold, and naturally leveling;
and a sixth step: curing at 60 ℃ for 3 days or curing at 70 ℃ for 2 days to obtain the toughening epoxy adhesive which can be reprocessed and recycled.
9. The method of claim 8 wherein the epoxy adhesive is a curable toughened epoxy adhesive which is reworkable and recyclable, the method comprising: the mixing method in the fourth step is that the mixing method in the fourth step is mechanical stirring dispersion, the stirring speed is 100-.
10. The method of claim 8 wherein the epoxy adhesive is a curable toughened epoxy adhesive which is reworkable and recyclable, the method comprising: the fifth step of centrifugal defoaming adopts a planetary gravity centrifugal defoaming machine, the revolution speed is 2000-3000r/min, the rotation speed is 1400-2100r/min, the time is 2-5min, and the temperature is room temperature.
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| CN114989562A (en) * | 2022-05-31 | 2022-09-02 | 西安热工研究院有限公司 | Recyclable metallographic insert and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114686149A (en) * | 2022-04-27 | 2022-07-01 | 广西至善新材料科技有限公司 | Reversible epoxy resin adhesive and preparation method thereof |
| CN114686149B (en) * | 2022-04-27 | 2023-10-20 | 广西至善新材料科技有限公司 | Reversible epoxy resin adhesive and preparation method thereof |
| CN114989562A (en) * | 2022-05-31 | 2022-09-02 | 西安热工研究院有限公司 | Recyclable metallographic insert and preparation method thereof |
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