CN115806791A - Medium-temperature fast-curing epoxy adhesive for switch products, preparation method and use method - Google Patents
Medium-temperature fast-curing epoxy adhesive for switch products, preparation method and use method Download PDFInfo
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- CN115806791A CN115806791A CN202111082710.XA CN202111082710A CN115806791A CN 115806791 A CN115806791 A CN 115806791A CN 202111082710 A CN202111082710 A CN 202111082710A CN 115806791 A CN115806791 A CN 115806791A
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Abstract
The invention discloses a medium-temperature fast-curing epoxy adhesive for switch products, a preparation method and a use method. The switch product is a medium-temperature fast curing epoxy adhesive. The epoxy adhesive consists of a component A and a component B; the component A consists of the following raw materials in parts by weight: 80-100 parts of bisphenol A type epoxy resin, 6-20 parts of reactive diluent and 0.1-1 part of silane coupling agent; the component B comprises the following raw materials in parts by weight: 24-30 parts of amine curing agent and 3-5 parts of accelerator. The invention has the beneficial effects that: the medium-temperature curing is realized, the curing time is short, the production takt of switch products is effectively shortened, and the method has wide application prospects in the electronic industry and aerospace.
Description
Technical Field
The invention relates to a medium-temperature fast curing epoxy adhesive for switch products, a preparation method and a use method thereof.
Background
The epoxy adhesive has excellent heat resistance, mechanical strength, insulating property and adhesion. Epoxy adhesives are widely used in the fields of aviation, aerospace, rail transit, construction and electronics industries, such as adhesives that are used in large quantities as housings in switching products within the above-mentioned fields. The disadvantages are that the curing temperature of the existing epoxy adhesive is higher, and the curing time is longer (generally, 24 hours is needed). With the gradual popularization of intelligent manufacturing, more and more switch products are changed from traditional manual operation to automatic production, and the longer curing time cannot meet the beat requirement of the automatic production of the switch products. Moreover, the tolerance temperature of the switch product is usually not more than 150 ℃, and a high-temperature accelerated curing type epoxy adhesive cannot be used.
Disclosure of Invention
The invention aims to solve the problems of high curing temperature and long curing time of epoxy adhesives in the prior art, and provides a novel medium-temperature fast curing epoxy adhesive for switch products, a preparation method and a use method.
In order to achieve the purpose, the technical scheme of the invention is as follows: the switch product is a medium-temperature fast curing epoxy adhesive, and the epoxy adhesive consists of a component A and a component B; the component A consists of the following raw materials in parts by weight: 80-100 parts of bisphenol A type epoxy resin, 6-20 parts of reactive diluent and 0.1-1 part of silane coupling agent; the component B consists of the following raw materials in parts by weight: 24-30 parts of amine curing agent and 3-5 parts of accelerator.
As a preferable scheme of the intermediate-temperature fast curing epoxy adhesive for switch products, the bisphenol A type epoxy resin is one or a mixture of more than two of epoxy resin E-51 (618), epoxy resin E-44 (6101) and other epoxy resins with the epoxy value of 0.20-0.56.
As a preferable scheme of the moderate-temperature fast curing epoxy adhesive for switch products, the reactive diluent is one or a mixture of more than two of 1, 4-butanediol diglycidyl ether 622, trihydroxymethyl triglycidyl ether 636 and 1, 6-hexanediol diglycidyl ether 632.
As a preferable scheme of the moderate-temperature fast curing epoxy adhesive for switch products, the silane coupling agent is one or a mixture of more than two of KH-550, KH-560 and KH-570.
As a preferable scheme of the moderate-temperature fast curing epoxy adhesive for switch products, the amine curing agent is an adduct of diethylenetriamine and butyl glycidyl ether.
As a preferable scheme of the intermediate-temperature fast curing epoxy adhesive for switch products, the accelerator is 2,4, 6-tris (dimethylaminomethyl) phenol, and can be one or a mixture of DMP-30 and K-54.
The invention also provides a preparation method of the medium-temperature fast curing epoxy adhesive for switch products, which is used for preparing the medium-temperature fast curing epoxy adhesive for switch products and comprises the following steps,
preparing a component A: heating bisphenol A epoxy resin to a thinning state, adding the bisphenol A epoxy resin, an active diluent and a silane coupling agent into a first stirring container, and uniformly stirring;
preparing a component B: firstly, adding the amine curing agent and the accelerator into a second stirring container together, stirring uniformly at normal temperature and normal pressure, and then vacuumizing the interior of the second stirring container until bubbles completely disappear.
As a preferred scheme of the preparation method of the intermediate-temperature fast curing epoxy adhesive for switch products, in the step of preparing the component A, the heating temperature of the bisphenol A type epoxy resin is 40-60 ℃, and the heating time is 1-2 hours.
The invention also provides a using method of the medium-temperature fast curing epoxy adhesive for switch products, which comprises the following steps,
providing the intermediate-temperature fast curing epoxy adhesive for the switch product; and the number of the first and second groups,
the component A and the component B are uniformly mixed according to the weight ratio of (2-3.5) to (1) and then are coated for use.
As a preferred scheme of the using method of the medium-temperature fast curing epoxy adhesive for switch products, the component A and the component B are uniformly mixed according to the weight ratio of 3.3.
Compared with the prior art, the invention has the beneficial effects that: the adhesive has stronger tensile shear strength to steel and aluminum materials and very good adhesive force to plastics, in particular to phenolic materials; the epoxy adhesive is primarily cured for 2min at the medium temperature of 100 ℃, the complete curing time is 5min, the curing time is 30min at the normal temperature, the cured ShoreD is 60-80, the color is colorless to light yellow and transparent, and the adhesive force is more than 30Mpa. The method is suitable for the mass production of switch products, can be used for quick joint filling, bonding, potting, insulation and the like, effectively shortens the production takt, and has wide application prospect in the electronic industry and aerospace.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. Here, the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 1g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
Mixing the component A and the component B according to a weight ratio of 3.3 to 1, coating the glue on a bonding sample according to GB/T7124, curing at a medium temperature of 100 ℃ for 5min by using a constant temperature box, and taking out the sample.
Example 2:
preparing a component A: 100g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 6g of reactive diluent 622 and 0.5g of silane coupling agent KH505 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 30g of amine curing agent 593 and 3g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (the stirring speed is 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (the vacuum time is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 3.
Example 3:
preparing a component A: 100g of epoxy resin E44 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 16g of reactive diluent 636 and 0.5g of silane coupling agent KH505 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 30g of amine curing agent 593 and 3g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed is 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 3.
Example 4:
preparing a component A: 90g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 16g of reactive diluent 622 and 0.5g of silane coupling agent KH505 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 30g of amine curing agent 593 and 3g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (K-54) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed is 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 3.
Comparative example 1:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature 40 ℃) to be in a diluted state and then added into a first stirring container together with 12g of reactive diluent 622 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (K-54) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed is 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
Mixing the component A and the component B according to a weight ratio of 3.3 to 1, coating the glue on a bonding sample according to GB/T7124, curing at medium temperature (100 ℃) for 5min by using a constant temperature box, and taking out the sample.
In comparative example 1, the silane coupling agent KH550 was not used, relative to example 1.
Comparative example 2:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 1g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 2.
Compared with the example 1, the component A and the component B of the comparative example 2 are mixed according to the weight ratio of 2.
Comparative example 3:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 1g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
Mixing the component A and the component B according to a weight ratio of 3.5 to 1, coating the glue on a bonding sample according to GB/T7124, curing at a medium temperature of 100 ℃ for 5min by using a constant temperature box, and taking out the sample.
Compared with the example 1, the component A and the component B in the comparative example 3 are mixed according to the weight ratio of 3.5.
Comparative example 4:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 1g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to the weight ratio of 1.
Compared with the example 1, the component A and the component B of the comparative example 4 are mixed according to the weight ratio of 1.
Comparative example 5:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a diluted state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 0.2g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 3.3.
The silane coupling agent KH550 of comparative example 5 was 0.2g, relative to example 1.
Comparative example 6:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a thinning state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 0.6g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
Mixing the component A and the component B according to a weight ratio of 3.3 to 1, coating the glue on a bonding sample according to GB/T7124, curing at a medium temperature of 100 ℃ for 5min by using a constant temperature box, and taking out the sample.
The silane coupling agent KH550 of comparative example 6 was 0.6g relative to example 1.
Comparative example 7:
preparing a component A: 85g of epoxy resin E51 is heated (heating temperature is 40 ℃) to be in a thinning state, and then is added into a first stirring container together with 12g of reactive diluent 622 and 1.4g of silane coupling agent KH550 to be uniformly stirred (stirring speed is 200r/min, and stirring time is 30 minutes).
Preparing a component B: firstly, 24g of amine curing agent 593 and 5g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure (stirring speed 100 r/min), and then the interior of the second stirring container is vacuumized until bubbles completely disappear (vacuum duration is 30 minutes).
And (3) mixing the component A and the component B according to a weight ratio of 3.3.
The silane coupling agent KH550 of comparative example 7 was 1.4g relative to example 1.
Commercial example 1:
commercially available two-component epoxy glue DP270 from 3M company, USA, was mixed according to the weight ratio 1.
And (3) test results:
the epoxy adhesives prepared in the examples 1-4, the comparative example 1 and the commercial example 1 are detected by a GB/T7124 adhesive shear strength measuring method, and the results are shown in the following table;
examples 1 to 4, commercial example 1 comparison: the shear strength, hardness and curing time of examples 1 to 4 were all significantly improved.
Examples 1 to 4, comparative example 1 compare: the shear strength and the hardness of the samples 1 to 4 are both remarkably improved, and the curing time is basically unchanged, namely, the silane coupling agent KH550 is added to effectively improve the shear strength and the hardness.
Example 1, comparative examples 2 to 4 compare: the shear strength and hardness of example 1 are superior to those of the other examples. The shear strength of comparative example 4 is significantly lower than the other examples. That is, it was revealed that the weight ratio of the A component to the B component had an influence on the shear strength and hardness, and the weight ratio was not as large as possible, but the weight ratio of example 1 was preferable.
Example 1, comparative examples 5 to 7: the shear strength of example 1 is superior to the other examples.
The foregoing merely represents embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The intermediate-temperature fast curing epoxy adhesive for switch products is characterized by comprising a component A and a component B; the component A consists of the following raw materials in parts by weight: 80-100 parts of bisphenol A type epoxy resin, 6-20 parts of reactive diluent and 0.1-1 part of silane coupling agent; the component B comprises the following raw materials in parts by weight: 24 to 30 parts of amine curing agent and 3 to 5 parts of accelerant.
2. The medium-temperature fast-curing epoxy adhesive for switch products according to claim 1, wherein the bisphenol a type epoxy resin is one or a mixture of any two or more of epoxy resin E-51 (618), epoxy resin E-44 (6101), and other epoxy resins with an epoxy value of 0.20-0.56.
3. The moderate temperature fast curing epoxy adhesive for switch products according to claim 1, wherein the reactive diluent is one or a mixture of any two or more of 1, 4-butanediol diglycidyl ether 622, trimethylol triglycidyl ether 636 and 1, 6-hexanediol diglycidyl ether 632.
4. The medium-temperature fast-curing epoxy adhesive for switch products as claimed in claim 1, wherein the silane coupling agent is one or a mixture of any two or more of KH-550, KH-560 and KH-570.
5. A moderate temperature fast curing epoxy adhesive for switch products according to claim 1, wherein the amine curing agent is an adduct of diethylenetriamine and butyl glycidyl ether.
6. An intermediate-temperature fast-curing epoxy adhesive for switch products as claimed in claim 1, wherein the accelerator is 2,4, 6-tris (dimethylaminomethyl) phenol, which may be one or a mixture of DMP-30 and K-54.
7. A preparation method of a medium-temperature fast curing epoxy adhesive for switch products, which is used for preparing the medium-temperature fast curing epoxy adhesive for switch products in any one of claims 1 to 6, is characterized by comprising the following steps of,
preparing a component A: heating bisphenol A epoxy resin to a thinning state, adding the bisphenol A epoxy resin, an active diluent and a silane coupling agent into a first stirring container, and uniformly stirring;
preparing a component B: the amine curing agent and the accelerator are added into a second stirring container together and stirred uniformly at normal temperature and normal pressure, and then the interior of the second stirring container is vacuumized until bubbles disappear completely.
8. The method for preparing the intermediate-temperature fast curing epoxy adhesive for the switch products according to claim 7, wherein in the step of preparing the component A, the heating temperature of the bisphenol A type epoxy resin is 40-60 ℃, and the heating time is 1-2 hours.
9. The application method of the intermediate-temperature fast curing epoxy adhesive for switch products is characterized by comprising the following steps of,
providing a medium temperature fast curing epoxy adhesive for a switching product according to any one of claims 1 to 6; and (c) a second step of,
the component A and the component B are uniformly mixed according to the weight ratio of (2-3.5) to (1) and then are coated for use.
10. The use method of the medium-temperature fast-curing epoxy adhesive for the switch product according to claim 9 is characterized in that the component A and the component B are uniformly mixed according to the weight ratio of 3.3 to 1 and then coated for use.
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