CN116445119A - Flexible insulating epoxy resin pouring sealant and preparation method thereof - Google Patents
Flexible insulating epoxy resin pouring sealant and preparation method thereof Download PDFInfo
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- CN116445119A CN116445119A CN202310576561.5A CN202310576561A CN116445119A CN 116445119 A CN116445119 A CN 116445119A CN 202310576561 A CN202310576561 A CN 202310576561A CN 116445119 A CN116445119 A CN 116445119A
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- epoxy resin
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- bisphenol
- flexible insulating
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 126
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 126
- 239000000565 sealant Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 39
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 28
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000003085 diluting agent Substances 0.000 claims abstract description 22
- 239000013530 defoamer Substances 0.000 claims abstract description 21
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 20
- 229920000570 polyether Polymers 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 150000001412 amines Chemical class 0.000 claims abstract description 19
- 239000011256 inorganic filler Substances 0.000 claims abstract description 19
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 19
- 239000000049 pigment Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims description 37
- 238000005303 weighing Methods 0.000 claims description 18
- 239000004593 Epoxy Substances 0.000 claims description 11
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004382 potting Methods 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- FUIQBJHUESBZNU-UHFFFAOYSA-N 2-[(dimethylazaniumyl)methyl]phenolate Chemical compound CN(C)CC1=CC=CC=C1O FUIQBJHUESBZNU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims 1
- -1 DMP-20 Chemical compound 0.000 claims 1
- 238000013329 compounding Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000002518 antifoaming agent Substances 0.000 description 7
- 238000009413 insulation Methods 0.000 description 6
- 150000008064 anhydrides Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005538 encapsulation Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical group C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical group CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a flexible insulating epoxy resin pouring sealant and a preparation method thereof, wherein the flexible insulating epoxy resin pouring sealant comprises a component A and a component B; the component A comprises the following preparation raw materials in parts by weight: 80-100 parts of bisphenol A epoxy resin, 5-10 parts of bisphenol F epoxy resin, 10-20 parts of flexible epoxy resin, 20-50 parts of inorganic filler, 10-20 parts of reactive diluent, 1-3 parts of defoamer, 1-3 parts of pigment and 1-3 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 95-100 parts of polyether amine curing agent; 1-3 parts of a promoter; the weight ratio of the component A to the component B is 3:1. The defects of high hardness, large brittleness, no flexibility and the like of the epoxy resin pouring sealant are overcome, the flexibility of the epoxy resin pouring sealant is increased, bisphenol F epoxy resin can be mixed with bisphenol A epoxy resin in a formula in any proportion, and the overall cost is reduced. Meanwhile, the encapsulating requirement on electronic product components can be met, the loss is reduced, the energy is saved, and the service life is prolonged.
Description
Technical Field
The invention relates to the technical field of pouring sealants, in particular to a flexible insulating epoxy resin pouring sealant and a preparation method thereof.
Background
With the development of science and technology, certain electronic component products need to be bent resistant after encapsulation, have flexibility, the flexible epoxy resin pouring sealant overcomes the defects of high hardness, large brittleness, no flexibility and the like of epoxy resin, has high and low temperature resistance, high insulation and high pressure resistance, good shock resistance and sealing performance, plays a very good role in protecting the encapsulation of electronic product components, meets various requirements of the encapsulation of the electronic product, reduces loss, saves energy, reduces equipment cost, prolongs service life, meets market demands, and solves the defects of high brittleness and easy breakage of the epoxy resin pouring sealant.
The invention discloses a high-flame-retardance epoxy resin pouring sealant with the application number of CN202010736422.0 and a preparation method thereof, wherein the high-flame-retardance epoxy resin pouring sealant comprises a component A and a component B, and the component A comprises the following components in parts by weight: 10-20 parts of polypropylene glycol diglycidyl ether, 4-8 parts of bisphenol A epoxy resin, 8-12 parts of trifunctional epoxy diluent, 0.5-2 parts of graphene oxide, 0.2-0.5 part of fumed silica, 10-16 parts of alpha-alumina powder and 40-60 parts of crystalline silica powder; the component B comprises: 3-8 parts of tertiary amine curing agent, 20-40 parts of organosilicon modified polyether amine and 50-80 parts of first polyether amine. The components are matched, so that the flame retardant and heat conductive adhesive has excellent flame retardance and heat conductive property, low viscosity, easy achievement of curing conditions, long normal-temperature operability time and good insulativity and mechanical property, and is particularly suitable for packaging electronic components.
However, the above disclosed high flame retardant epoxy resin pouring sealant cannot meet the demands of customers in terms of flexibility, and meanwhile, the manufacturing cost is high, and we need to find an epoxy resin pouring sealant with high flexibility, insulation and low cost to meet the market demands.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide the flexible insulating epoxy resin pouring sealant, which can effectively solve the technical problems of poor flexibility and high preparation cost of the epoxy resin pouring sealant for electronic products in the prior art. Meanwhile, the invention also provides a preparation method of the flexible insulating epoxy resin pouring sealant.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a flexible insulating epoxy potting adhesive, comprising a component a and a component B;
the component A comprises the following preparation raw materials in parts by weight: 80-100 parts of bisphenol A epoxy resin, 5-10 parts of bisphenol F epoxy resin, 10-20 parts of flexible epoxy resin, 20-50 parts of inorganic filler, 10-20 parts of reactive diluent, 1-3 parts of defoamer, 1-3 parts of pigment and 1-3 parts of auxiliary agent;
the component B comprises the following preparation raw materials in parts by weight: 95-100 parts of polyether amine curing agent; 1-3 parts of a promoter;
the weight ratio of the component A to the component B is 3:1.
Specifically, the bisphenol A epoxy resin is E-51 epoxy resin and/or E-44 epoxy resin.
Preferably, the flexible epoxy resin is produced by Kogyo New Material technology Co., ltd in Dongguan, and has the product model number ZK-1828.
Preferably, the bisphenol A epoxy resin is E-51 epoxy resin and/or E-44 epoxy resin.
Preferably, the reactive diluent is methyltetrahydrophthalic anhydride and/or methylhexahydrophthalic anhydride.
Preferably, the defoamer is BYK1795 and/or TSA750S.
Preferably, the auxiliary agent is one or a mixture of a plurality of gamma-aminopropyl triethoxysilane, gamma-glycidoxy trimethoxysilane and gamma-aminopropyl trimethoxysilane.
Preferably, the accelerator is one or a mixture of several of DMP-10, DMP-20 and DMP-30.
Preferably, the bisphenol F epoxy resin is F-51 epoxy resin and/or F-44 epoxy resin.
Preferably, the preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, bisphenol F epoxy resin, flexible epoxy resin, reactive diluent, inorganic filler, defoamer, pigment and auxiliary agent in the component A according to a formula, adding the weighed components into a dispersion stirrer, carrying out dispersion stirring for 0.5-1.5h at the speed of 800-1500rpm at normal temperature, and then vacuumizing the dispersion stirrer to-0.097 to-0.1 Mpa, and continuing the dispersion stirring for 1-2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyether amine curing agent and the accelerator in the component B according to a formula, adding the components into another dispersing stirrer, heating to 30-40 ℃, vacuumizing the dispersing stirrer to-0.097 to-0.1 Mpa, and dispersing and stirring for 0.3-0.5h at a stirring rate of 500-1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
The application method of the flexible insulating epoxy resin pouring sealant comprises the steps of mixing the component A and the component B according to the weight ratio of 3:1, curing at normal temperature, and curing within the operation time of 60-90min and 24-48 h; and obtaining the flexible insulating epoxy resin pouring sealant.
In the formula, the flexible epoxy resin is added to overcome the defects of high hardness, large brittleness, no flexibility and the like of the epoxy resin pouring sealant, and the flexibility of the epoxy resin pouring sealant is increased. The flexible epoxy resin is toughened and modified epoxy resin, and a high boiling point compound of a short molecular chain or a flexible chain is added into the epoxy resin to reduce the potential barrier of chain movement between crosslinking points of a cured product, and the interaction between a base material macromolecular chain segment and a small molecule is utilized to replace the interaction between macromolecular chain segments, so that the flexibility is improved, the flexibility is endowed, and the extensibility and the impact toughness are improved.
Meanwhile, bisphenol F epoxy resin is added in the formula, the viscosity is low, the epoxy resin can be mixed with bisphenol A epoxy resin in the formula in any proportion, the viscosity is reduced to less than 1/3 of the viscosity of the bisphenol A epoxy resin, the overall viscosity is reduced by matching with the epoxy resin, the crystallization trend is also cancelled, and meanwhile, the flexibility can be improved. Other performances are the same as those of bisphenol A epoxy resin, and the addition of the bisphenol A epoxy resin can reduce the overall cost without affecting other mechanical properties.
In the formula, polyether amine curing agents are used instead of anhydride curing agents, and compared with the polyether amine curing agents, the polyether amine curing agents have more flexible groups such as methylene (C-I) ether bond (-O-I) and the like in the molecular structure, the flexible chain segments can be bonded into a compact epoxy resin crosslinked network, microscopic phase separation is generated in the curing process, a two-phase network structure between compact phases and loose phases is formed, the polyether main chain imparts flexibility, the polyvinyl alcohol imparts hydrophilicity and amine-terminated reactivity, and the polyvinyl alcohol imparts biocompatibility. The color and luster are light, the viscosity is low, the stability is good, the brightness is high, and the leveling property is good; the flexibility of the epoxy resin pouring sealant can be increased due to the characteristic of good flexibility after solidification.
The flexible insulating epoxy resin pouring sealant and one or more technical schemes in the preparation thereof provided by the embodiment of the invention have at least one of the following technical effects:
the flexible insulating epoxy resin pouring sealant overcomes the defects of high hardness, large brittleness, no flexibility and the like of the epoxy resin pouring sealant, increases the flexibility of the epoxy resin pouring sealant, can be mixed with bisphenol A epoxy resin in a formula in any proportion, reduces the viscosity, eliminates the crystallization trend, can improve the flexibility at the same time, has the same other performances as the bisphenol A epoxy resin, and can reduce the overall cost by adding the bisphenol A epoxy resin. Meanwhile, the encapsulating requirement on electronic product components can be met, the loss is reduced, the energy is saved, and the service life is prolonged.
Detailed Description
For better illustrating the objects, technical solutions and advantageous effects of the present invention, the present invention will be further described with reference to specific embodiments.
Example 1
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 80 parts of bisphenol A epoxy resin, 10 parts of bisphenol F epoxy resin, 20 parts of flexible epoxy resin, 50 parts of inorganic filler, 20 parts of reactive diluent, 3 parts of defoamer, 3 parts of pigment and 3 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 95 parts of polyether amine curing agent; 3 parts of a promoter; the weight ratio of the component A to the component B is 3:1.
The flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is a mixture of E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the accelerator is a mixture of DMP-10, DMP-20 and DMP-30; the bisphenol F epoxy resin is F-51 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, bisphenol F epoxy resin, flexible epoxy resin, reactive diluent, inorganic filler, defoamer, pigment and auxiliary agent in the component A according to a formula, adding the weighed components into a dispersing stirrer, dispersing and stirring for 1h at the speed of 1000rpm at normal temperature, vacuumizing the dispersing stirrer to-0.1 Mpa, and continuing dispersing and stirring for 1h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyether amine curing agent and the accelerator in the component B according to a formula, adding the components into another dispersing stirrer, heating to 40 ℃, vacuumizing the dispersing stirrer to-0.1 Mpa, and dispersing and stirring for 0.4h at a stirring speed of 800rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Example 2
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 90 parts of bisphenol A epoxy resin, 15 parts of bisphenol F epoxy resin, 18 parts of flexible epoxy resin, 30 parts of inorganic filler, 15 parts of reactive diluent, 2 parts of defoamer, 2 parts of pigment and 2 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 98 parts of polyether amine curing agent; 2 parts of accelerator; the weight ratio of the component A to the component B is 3:1.
The flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the accelerator is DMP-30; the bisphenol F epoxy resin is F-51 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing the bisphenol A epoxy resin, the bisphenol F epoxy resin, the flexible epoxy resin, the reactive diluent, the inorganic filler, the defoamer, the pigment and the auxiliary agent in the component A according to a formula, adding the components into a dispersing mixer, stirring at 1000rpm at normal temperature for 1h, starting vacuum at-0.1 Mpa, and continuing to disperse and stir for 2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyetheramine curing agent and the accelerator in the component B according to a formula, adding the components into a dispersing mixer, heating to 30 ℃, then starting vacuum under-0.1 Mpa, and dispersing and stirring for 0.5h at a stirring speed of 1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Example 3
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 92 parts of bisphenol A epoxy resin, 7 parts of bisphenol F epoxy resin, 15 parts of flexible epoxy resin, 35 parts of inorganic filler, 17 parts of reactive diluent, 2 parts of defoamer, 2 parts of pigment and 2 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 97 parts of polyether amine curing agent; 2 parts of accelerator; the weight ratio of the component A to the component B is 3:1.
The flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the accelerator is DMP-30; the bisphenol F epoxy resin is F-44 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, bisphenol F epoxy resin, flexible epoxy resin, reactive diluent, inorganic filler, defoamer, pigment and auxiliary agent in the component A according to a formula, adding the weighed components into a dispersing stirrer, dispersing and stirring for 1h at the speed of 1000rpm at normal temperature, vacuumizing the dispersing stirrer to-0.1 Mpa, and continuing dispersing and stirring for 1h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyether amine curing agent and the accelerator in the component B according to a formula, adding the components into another dispersing stirrer, heating to 40 ℃, vacuumizing the dispersing stirrer to-0.1 Mpa, and dispersing and stirring for 0.4h at a stirring speed of 800rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Example 4
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 100 parts of bisphenol A epoxy resin, 5 parts of bisphenol F epoxy resin, 10 parts of flexible epoxy resin, 20 parts of inorganic filler, 10 parts of reactive diluent, 1 part of defoamer, 1 part of pigment and 1 part of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 100 parts of polyether amine curing agent; 1 part of accelerator; the weight ratio of the component A to the component B is 3:1.
The flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-glycidoxy trimethoxy silane; the accelerator is DMP-30; the bisphenol F epoxy resin is F-51 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, bisphenol F epoxy resin, flexible epoxy resin, reactive diluent, inorganic filler, defoamer, pigment and auxiliary agent in the component A according to a formula, adding the weighed components into a dispersing stirrer, dispersing and stirring for 1h at the speed of 1000rpm at normal temperature, vacuumizing the dispersing stirrer to-0.1 Mpa, and continuing dispersing and stirring for 1h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyether amine curing agent and the accelerator in the component B according to a formula, adding the components into another dispersing stirrer, heating to 40 ℃, vacuumizing the dispersing stirrer to-0.1 Mpa, and dispersing and stirring for 0.4h at a stirring speed of 800rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Comparative example 1
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 90 parts of bisphenol A epoxy resin, 15 parts of bisphenol F epoxy resin, 30 parts of inorganic filler, 15 parts of reactive diluent, 2 parts of defoamer, 2 parts of pigment and 2 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 98 parts of polyether amine curing agent; 2 parts of accelerator; the weight ratio of the component A to the component B is 3:1.
The bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the accelerator is DMP-30; the bisphenol F epoxy resin is F-51 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing the bisphenol A epoxy resin, the bisphenol F epoxy resin, the reactive diluent, the inorganic filler, the defoamer, the pigment and the auxiliary agent in the component A according to a formula, adding the components into a dispersing mixer, stirring at normal temperature at 1000rpm, dispersing and stirring for 1h, and then starting vacuum under-0.1 Mpa, and continuing dispersing and stirring for 2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyetheramine curing agent and the accelerator in the component B according to a formula, adding the components into a dispersing mixer, heating to 30 ℃, then starting vacuum under-0.1 Mpa, and dispersing and stirring for 0.5h at a stirring speed of 1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Comparative example 2
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 90 parts of bisphenol A epoxy resin, 18 parts of flexible epoxy resin, 30 parts of inorganic filler, 15 parts of reactive diluent, 2 parts of defoamer, 2 parts of pigment and 2 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 98 parts of polyether amine curing agent; 2 parts of accelerator; the weight ratio of the component A to the component B is 3:1.
The flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the promoter is DMP-30.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, flexible epoxy resin, the reactive diluent, the inorganic filler, the defoamer, the pigment and the auxiliary agent in the component A according to a formula, adding the components into a dispersing mixer, stirring at 1000rpm at normal temperature for 1h, and then starting vacuum under-0.1 Mpa for continuous dispersing and stirring for 2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyetheramine curing agent and the accelerator in the component B according to a formula, adding the components into a dispersing mixer, heating to 30 ℃, then starting vacuum under-0.1 Mpa, and dispersing and stirring for 0.5h at a stirring speed of 1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
Comparative example 3
A flexible insulating epoxy resin pouring sealant comprises a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 90 parts of bisphenol A epoxy resin, 15 parts of bisphenol F epoxy resin, 18 parts of flexible epoxy resin, 30 parts of inorganic filler, 15 parts of reactive diluent, 2 parts of defoamer, 2 parts of pigment and 2 parts of auxiliary agent; the component B comprises the following preparation raw materials in parts by weight: 98 parts of anhydride curing agent; 2 parts of accelerator; the weight ratio of the component A to the component B is 3:1.
The anhydride curing agent is methyl tetrahydrophthalic anhydride curing agent, and the flexible epoxy resin is ZK-1828; the bisphenol A epoxy resin is E-51 epoxy resin and E-44 epoxy resin; the defoaming agent is BYK1795; the auxiliary agent is gamma-aminopropyl triethoxysilane; the promoter is Benzyl Dimethylamine (BDMA); the bisphenol F epoxy resin is F-51 epoxy resin.
The preparation method of the flexible insulating epoxy resin pouring sealant comprises the following steps:
preparing a component A:
respectively weighing the bisphenol A epoxy resin, the bisphenol F epoxy resin, the flexible epoxy resin, the reactive diluent, the inorganic filler, the defoamer, the pigment and the auxiliary agent in the component A according to a formula, adding the components into a dispersing mixer, stirring at 1000rpm at normal temperature for 1h, starting vacuum at-0.1 Mpa, and continuing to disperse and stir for 2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the anhydride curing agent and the accelerator in the component B according to a formula, adding the anhydride curing agent and the accelerator into a dispersing mixer, heating to 30 ℃, then starting vacuum under-0.1 Mpa, and dispersing and stirring for 0.5h at a stirring speed of 1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
the component A and the component B are mixed according to the proportion of 3:1 to obtain the flexible insulating epoxy resin pouring sealant.
The rest of the present embodiment is the same as the first embodiment, and the unexplained features in the present embodiment are all explained by the first embodiment, and are not described here again.
The flexible insulating epoxy resin pouring sealant in the examples 1-4 and the comparative examples 1-3 are subjected to unified experimental comparison, the Shore A hardness is measured by using a TIME5430 digital display Shore A hardness tester according to the reference GB/T531-1999, and the elongation at break and the tensile strength are measured by using a universal tensile machine according to the reference GB/T1040.1-2006; the cold and hot impact properties were measured with a cold and hot impact box at-40 c/1 h to 120 c/1 h for 100 cycles, the use temperature range was determined according to the cold and hot impact properties, and the occurrence of cracking was regarded as unusable, the volume resistivity was measured according to ASTM D257 using an insulation resistance tester and the volume resistivity was calculated, the insulation strength was measured using an insulation strength tester, and the test results are shown in table 1.
TABLE 1
As can be seen from the results in Table 1, the flexible insulating epoxy resin pouring sealants of examples 1 to 4 and comparative examples 1 to 3 of the present invention have good mechanical properties, and simultaneously have good flexibility, cold and hot impact resistance, high tensile strength, stretch resistance, insulation and high and low temperature resistance.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The flexible insulating epoxy resin pouring sealant is characterized by comprising a component A and a component B;
the component A comprises the following preparation raw materials in parts by weight: 80-100 parts of bisphenol A epoxy resin, 5-10 parts of bisphenol F epoxy resin, 10-20 parts of flexible epoxy resin, 20-50 parts of inorganic filler, 10-20 parts of reactive diluent, 1-3 parts of defoamer, 1-3 parts of pigment and 1-3 parts of auxiliary agent;
the component B comprises the following preparation raw materials in parts by weight: 95-100 parts of polyether amine curing agent; 1-3 parts of a promoter;
the weight ratio of the component A to the component B is 3:1.
2. The flexible insulating epoxy potting adhesive of claim 1, wherein the bisphenol a epoxy resin is an E-51 epoxy resin and/or an E-44 epoxy resin.
3. The flexible insulating epoxy potting adhesive of claim 1, wherein the flexible epoxy is produced by the industry of new materials technology, inc. of Kogyo in Dongguan, product model number ZK-1828.
4. The flexible insulating epoxy potting adhesive of claim 1, wherein the bisphenol a epoxy resin is an E-51 epoxy resin and/or an E-44 epoxy resin.
5. The flexible insulating epoxy potting adhesive of claim 1, wherein the reactive diluent is polypropylene glycol diglycidyl ether and/or butyl glycidyl ether.
6. The flexible insulating epoxy potting adhesive of claim 1, wherein the defoamer is BYK1795 and/or TSA750S.
7. The flexible insulating epoxy potting adhesive of claim 1, wherein the auxiliary agent is one or a mixture of a plurality of gamma-aminopropyl triethoxysilane, gamma-glycidoxy trimethoxysilane and gamma-aminopropyl trimethoxysilane.
8. The flexible insulating epoxy potting adhesive of claim 1, wherein the accelerator is one or a mixture of several of DMP-10, DMP-20, and DMP-30.
9. The flexible insulating epoxy potting adhesive of claim 1, wherein the bisphenol F epoxy resin is F-51 epoxy resin and/or F-44 epoxy resin.
10. A method for preparing the flexible insulating epoxy resin pouring sealant according to any one of claims 1 to 9, comprising the following steps:
preparing a component A:
respectively weighing bisphenol A epoxy resin, bisphenol F epoxy resin, flexible epoxy resin, reactive diluent, inorganic filler, defoamer, pigment and auxiliary agent in the component A according to a formula, adding the weighed components into a dispersion stirrer, carrying out dispersion stirring for 0.5-1.5h at the speed of 800-1500rpm at normal temperature, and then vacuumizing the dispersion stirrer to-0.097 to-0.1 Mpa, and continuing the dispersion stirring for 1-2h to obtain the component A;
and (3) preparing a component B:
respectively weighing the polyether amine curing agent and the accelerator in the component B according to a formula, adding the components into another dispersing stirrer, heating to 30-40 ℃, vacuumizing the dispersing stirrer to-0.097 to-0.1 Mpa, and dispersing and stirring for 0.3-0.5h at a stirring rate of 500-1000rpm to obtain the component B;
preparing flexible insulating epoxy resin pouring sealant:
and (3) mixing the component A and the component B according to the following weight ratio of 3: and (3) compounding the components according to the weight ratio of 1 to obtain the flexible insulating epoxy resin pouring sealant.
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