A hot-pressed magnetic powder connection adhesive and its preparation method

Abstract

The present invention discloses a hot-pressing magnetic powder connecting adhesive and a preparation method thereof, belonging to the technical field of connecting adhesives, and comprising the following components in percentage by weight: 45-65% fluorine-containing modified epoxy resin, 15-20% curing agent, 20-30% filler, 5-8% toughening agent, 0.5-1.5% auxiliary agent; the fluorine-containing modified epoxy resin is obtained by reacting bisphenol A epoxy resin with perfluorooctyltriethoxysilane, and the mass ratio of bisphenol A epoxy resin to perfluorooctyltriethoxysilane is (8-5):1. The hot-pressing magnetic powder connecting adhesive of the present invention has extremely high Tg and Td, can work stably at 280°C for a long time, is significantly superior to existing products (such as DM-6997), and meets the magnetic powder connection and insulation requirements in high-temperature scenarios such as oil drilling.

Description

Technical Field

[0001] The present invention relates to the technical field of connection adhesives, and particularly relates to a hot-pressing magnetic powder connection adhesive and a preparation method thereof. Background Art

[0002] The manufacture of integrally formed die piezoelectric inductors relies on a hot-pressing magnetic powder connection adhesive to insulate and coat magnetic powder particles and assemble them with coils and then hot-press them into shape. Taking the conventional DM-6997 adhesive on the market as an example, DM-6997 adhesive is a two-component epoxy resin-based adhesive (component A is a transparent epoxy resin solution, and component B is an off-white curing agent), which has excellent insulation and adhesiveness. The mixing mass ratio is 30:1, and the curing condition is 1 hour at 150°C. Its main properties include: glass transition temperature (Tg) of 110°C, cracking temperature (Td, 5% weight loss) of 275°C, and tensile shear strength greater than 8.0 MPa. However, the Tg of this adhesive is relatively low (110°C), and the long-term working temperature is limited to below 125°C, which cannot meet the requirements of extreme high-temperature environments (220 - 260°C or even higher) such as oil drilling. In addition, its reliability test only covers the range of -55~125°C, and the stability has not been verified at higher temperatures.

[0003] With the increasing requirements of special industries for the temperature resistance performance of inductors, the existing hot-pressing magnetic powder connection insulating adhesives are prone to cracking or splitting at high temperatures, resulting in the failure of inductors.

[0004] In view of this, the present application is proposed. Summary of the Invention

[0005] The purpose of the present invention is to overcome the deficiencies of the existing technology and provide a hot-pressing magnetic powder connection adhesive and a preparation method thereof. The hot-pressing magnetic powder connection adhesive of the present invention has extremely high Tg and Td, can work stably at 280°C for a long time, is significantly superior to existing products (such as DM-6997), and meets the magnetic powder connection and insulation requirements in high-temperature scenarios such as oil drilling.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0007] A hot-pressing magnetic powder connection adhesive, comprising the following components in weight percentage: 45~65% fluorine-modified epoxy resin, 15~20% curing agent, 20~30% filler, 5~8% toughening agent, 0.5~1.5% auxiliary agent;

[0008] The fluorine-modified epoxy resin is obtained by reacting bisphenol A epoxy resin with perfluorooctyltriethoxysilane, and the mass ratio of bisphenol A epoxy resin to perfluorooctyltriethoxysilane is (8~5):1

[0009] The curing agent comprises 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine with a mass ratio of 1:(0.5~2);

[0010] The filler comprises wollastonite fiber and flaky carbonyl iron powder in a mass ratio of 1:(0.5-2).

[0011] As a preferred embodiment of the present invention, the cashew nut shell oil phenol aldehyde amine has a viscosity of 2300-2500 cPs at 25° C. and an amine value of 340-390 mgKOH / g.

[0012] As a preferred embodiment of the present invention, the aspect ratio of the flaky carbonyl iron powder is (8-10):1.

[0013] As a preferred embodiment of the present invention, the aspect ratio of the wollastonite fiber is (12-15):1.

[0014] As a preferred embodiment of the present invention, the epoxy equivalent of the bisphenol A epoxy resin is 625-675 g / eq.

[0015] As a preferred embodiment of the present invention, the preparation method of the fluorine-containing modified epoxy resin is: bisphenol A epoxy resin and perfluorooctyltriethoxysilane are uniformly mixed, a catalyst is added, and the mixture is reacted to obtain the fluorine-containing modified epoxy resin.

[0016] As a preferred embodiment of the present invention, the catalyst is tetrabutyl titanate, and the mass ratio of the bisphenol A epoxy resin to the catalyst is 100: (0.1~1);

[0017] The reaction temperature is 75-95° C., and the reaction time is 2-8 hours.

[0018] As a preferred embodiment of the present invention, the toughening agent is polyetheramine.

[0019] As a preferred embodiment of the present invention, the auxiliary agent includes at least one of a defoaming agent and a leveling agent.

[0020] The present invention also provides a method for preparing a hot-pressed magnetic powder bonding adhesive, comprising the following steps:

[0021] The fluorine-containing modified epoxy resin, curing agent, filler, toughening agent and auxiliary agent are mixed evenly to obtain the hot-pressed magnetic powder connecting adhesive.

[0022] The beneficial effects of the present invention are as follows: (1) In the present invention, a fluorine-modified epoxy resin obtained by reacting bisphenol A epoxy resin with perfluorooctyltriethoxysilane is used as the main resin, and the thermal stability and chemical resistance of the fluorine-modified epoxy resin are significantly improved. (2) By optimizing bisphenol A epoxy resin and the curing agent, the crosslinking density and thermal stability are further improved, so that the hot-pressed magnetic powder connection adhesive has an extremely high Tg and Td, can work stably at 280 °C for a long time, is significantly superior to existing products (such as DM-6997), and meets the magnetic powder connection and insulation requirements in high-temperature scenarios such as oil drilling; (3) Wollastonite fibers and flaky carbonyl iron powder with a mass ratio of 1: (0.5 - 2) are used as fillers in the present invention. The wollastonite fibers and flaky carbonyl iron powder are interlaced with each other, can form a dense filling network structure in the system, and have a certain magnetic property, restricting the movement of polymer segments, effectively improving the thermal stability of the system, effectively increasing Tg and Td, and improving the bonding performance. Detailed Embodiments

[0023] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Apparently, the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative efforts shall fall within the scope of protection of the present application.

[0024] In the present application, for the technical features described in an open-ended manner, a closed technical solution composed of the listed features is included, and an open technical solution including the listed features is also included.

[0025] In the present application, regarding the numerical range, unless otherwise specified, the above numerical range is considered continuous and includes the minimum value and the maximum value of the range, as well as each value between such minimum value and maximum value. Further, when the range refers to an integer, each integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein.

[0026] In the present application, there are no particular restrictions on the specific dispersion and stirring treatment methods.

[0027] Unless otherwise specified, the component raw materials or instruments used in the embodiments and comparative examples of the present invention are all commercially available raw materials or instruments, and the component raw materials used in each parallel experiment are the same.

[0028] Among them, the raw materials of the examples and comparative examples are as follows:

[0029] Bisphenol A epoxy resin - 1: Epoxy equivalent weight is 625 - 675 g / eq, Shanghai Kayin Chemical Industry, grade epoxy resin KD - 242GHF.

[0030] Bisphenol A epoxy resin - 2: Epoxy equivalent weight is 875 - 975 g / eq, Shanghai Kayin Chemical Industry, grade epoxy resin KD - 214C.

[0031] Bisphenol A epoxy resin - 3, Epoxy equivalent weight is 405 - 450 g / eq, Shanghai Kayin Chemical Industry, grade epoxy resin KD - 211SW.

[0032] Cardanol - aldehyde - amine - 1: Viscosity at 25°C is 2500 cPs, amine value is 390 mgKOH / g, Cardolite, grade NX - 5352.

[0033] Cardanol - aldehyde - amine - 2: Viscosity at 25°C is 2300 cPs, amine value is 340 mgKOH / g, Cardolite, grade NX - 541LV.

[0034] Cardanol - aldehyde - amine - 3: Viscosity at 25°C is 770 cPs, amine value is 561 mgKOH / g, Cardolite, grade NX - 5567.

[0035] Cardanol - aldehyde - amine - 4: Viscosity at 25°C is 25000 cPs, amine value is 130 mgKOH / g, Cardolite, grade NC - 641.

[0036] Flaky carbonyl iron powder - 1: Aspect ratio (thickness to diameter) is 10:1, Xinxiang Sanyi New Materials, grade PF - 01.

[0037] Flaky carbonyl iron powder - 2: Aspect ratio (thickness to diameter) is 8:1, Xinxiang Sanyi New Materials, grade PF - 02.

[0038] Flaky carbonyl iron powder - 3: Aspect ratio (thickness to diameter) is 20:1, Xinxiang Sanyi New Materials, grade PF - 04.

[0039] Flaky carbonyl iron powder - 4: Aspect ratio (thickness to diameter) is 5:1, Xinxiang Sanyi New Materials, grade PF - 03.

[0040] Wollastonite fiber - 1: Aspect ratio (length to diameter) is 12:1, Fengjiashan Silicon Fiber Co., Ltd., grade WFA50.

[0041] Wollastonite fiber - 2: Aspect ratio (length to diameter) is 15:1, Fengjiashan Silicon Fiber Co., Ltd., grade WFA60.

[0042] Wollastonite fiber - 3: Aspect ratio (length to diameter) is 20:1, Fengjiashan Silicon Fiber Co., Ltd., grade WFA80.

[0043] Wollastonite fiber - 4: Aspect ratio 9:1, Fengjiashan Silicon Fiber Co., Ltd., grade WFB5.

[0044] Polyetheramine: Macklin reagent, D - 230.

[0045] Defoamer: BYK028 from BYK.

[0046] The following examples are provided to facilitate the understanding of the present invention. These examples are not provided to limit the scope of the claims.

[0047] Example 1

[0048] A hot - pressed magnetic powder connecting adhesive, comprising the following components by weight percentage: 51% fluorine - modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoamer.

[0049] The filler includes wollastonite fiber - 1 and flaky carbonyl iron powder - 1 with a mass ratio of 1:0.5.

[0050] The preparation method of the fluorine - modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin - 1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine - modified epoxy resin.

[0051] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine - 1 with a mass ratio of 1:2.

[0052] The preparation method of the hot - pressed magnetic powder connecting adhesive includes the following steps:

[0053] Mix the fluorine - modified epoxy resin, curing agent, filler, polyetheramine, and defoamer evenly to obtain the hot - pressed magnetic powder connecting adhesive.

[0054] Example 2

[0055] A hot - pressed magnetic powder connecting adhesive, comprising the following components by weight percentage: 48.5% fluorine - modified epoxy resin, 15% curing agent, 28% filler, 8% polyetheramine, 0.5% defoamer.

[0056] The filler includes wollastonite fiber - 1 and flaky carbonyl iron powder - 1 with a mass ratio of 1:0.5.

[0057] The preparation method of the fluorine - modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin - 1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine - modified epoxy resin.

[0058] The curing agent includes 4,4'-diaminodiphenyl sulfone and cardanol phenolic aldehyde amine-1 with a mass ratio of 1:2.

[0059] The preparation method of the hot pressing magnetic powder connecting adhesive includes the following steps:

[0060] Mix the fluorine-containing modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot pressing magnetic powder connecting adhesive.

[0061] Example 3

[0062] A hot pressing magnetic powder connecting adhesive includes the following components by weight percentage: 51% fluorine-containing modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, and 1% defoaming agent.

[0063] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0064] The preparation method of the fluorine-containing modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-2 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-containing modified epoxy resin.

[0065] The curing agent includes 4,4'-diaminodiphenyl sulfone and cardanol phenolic aldehyde amine-1 with a mass ratio of 1:2.

[0066] The preparation method of the hot pressing magnetic powder connecting adhesive includes the following steps:

[0067] Mix the fluorine-containing modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot pressing magnetic powder connecting adhesive.

[0068] Example 4

[0069] A hot pressing magnetic powder connecting adhesive includes the following components by weight percentage: 51% fluorine-containing modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, and 1% defoaming agent.

[0070] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0071] The preparation method of the fluorine-containing modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-3 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-containing modified epoxy resin.

[0072] The curing agent includes 4,4'-diaminodiphenyl sulfone and cardanol phenolic aldehyde amine-1 with a mass ratio of 1:2.

[0073] The preparation method of the hot-pressing magnetic powder connecting adhesive comprises the following steps:

[0074] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine and defoamer uniformly to obtain the hot-pressing magnetic powder connecting adhesive.

[0075] Example 5

[0076] A hot-pressing magnetic powder connecting adhesive comprises the following components in percentage by weight: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine and 1% defoamer.

[0077] The filler comprises wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:2.

[0078] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane uniformly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0079] The curing agent comprises 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:0.5.

[0080] The preparation method of the hot-pressing magnetic powder connecting adhesive comprises the following steps:

[0081] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine and defoamer uniformly to obtain the hot-pressing magnetic powder connecting adhesive.

[0082] Example 6

[0083] A hot-pressing magnetic powder connecting adhesive comprises the following components in percentage by weight: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine and 1% defoamer.

[0084] The filler comprises wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0085] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane uniformly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0086] The curing agent comprises 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-2 with a mass ratio of 1:2.

[0087] The preparation method of the hot-pressing magnetic powder connecting adhesive comprises the following steps:

[0088] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoamer evenly to obtain the hot-pressing magnetic powder connecting adhesive described above.

[0089] Example 7

[0090] A hot-pressing magnetic powder connecting adhesive includes the following components in weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, and 1% defoamer.

[0091] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0092] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0093] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-3 with a mass ratio of 1:2.

[0094] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0095] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoamer evenly to obtain the hot-pressing magnetic powder connecting adhesive described above.

[0096] Example 8

[0097] A hot-pressing magnetic powder connecting adhesive includes the following components in weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, and 1% defoamer.

[0098] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0099] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0100] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-4 with a mass ratio of 1:2.

[0101] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0102] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoamer evenly to obtain the hot-pressing magnetic powder connecting adhesive described above.

[0103] Example 9

[0104] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0105] The filler includes wollastonite fiber-2 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0106] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0107] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0108] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0109] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0110] Example 10

[0111] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0112] The filler includes wollastonite fiber-3 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0113] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0114] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0115] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0116] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0117] Example 11

[0118] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0119] The filler includes wollastonite fiber-4 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0120] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0121] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0122] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0123] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0124] Example 12

[0125] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0126] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-2 with a mass ratio of 1:0.5.

[0127] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0128] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0129] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0130] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0131] Example 13

[0132] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0133] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-3 with a mass ratio of 1:0.5.

[0134] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0135] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0136] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0137] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0138] Example 14

[0139] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0140] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-4 with a mass ratio of 1:0.5.

[0141] The preparation method of the fluorine-modified epoxy resin is as follows: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0142] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0143] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0144] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0145] Comparative Example 1

[0146] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% bisphenol A epoxy resin-1, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0147] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0148] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0149] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0150] Mix bisphenol A epoxy resin-1, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0151] Comparative Example 2

[0152] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0153] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0154] The preparation method of the fluorine-modified epoxy resin is: Mix 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane evenly, add 0.5 g of tetrabutyl titanate, and stir and react at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0155] The curing agent is 4,4'-diaminodiphenyl sulfone.

[0156] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0157] Mix the fluorine-modified epoxy resin, curing agent, filler, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0158] Comparative Example 3

[0159] A hot-pressing magnetic powder connecting adhesive, comprising components in the following weight percentages: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, 1% defoaming agent.

[0160] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0161] The preparation method of the fluorine-modified epoxy resin is as follows: 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane are mixed evenly, 0.5 g of tetrabutyl titanate is added, and the mixture is stirred and reacted at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0162] The curing agent is cashew shell oil phenolic amine-1.

[0163] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0164] The fluorine-modified epoxy resin, the curing agent, the filler, the polyetheramine, and the defoaming agent are mixed evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0165] Comparative Example 4

[0166] A hot-pressing magnetic powder connecting adhesive includes the following components by weight percentage: 51% fluorine-modified epoxy resin, 18% curing agent, 25% filler, 6% polyetheramine, and 1% defoaming agent.

[0167] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0168] The preparation method of the fluorine-modified epoxy resin is as follows: 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane are mixed evenly, 0.5 g of tetrabutyl titanate is added, and the mixture is stirred and reacted at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0169] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:0.25.

[0170] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0171] The fluorine-modified epoxy resin, the curing agent, the filler, the polyetheramine, and the defoaming agent are mixed evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0172] Comparative Example 5

[0173] A hot-pressing magnetic powder connecting adhesive includes the following components by weight percentage: 51% fluorine-modified epoxy resin, 18% curing agent, 24% filler, 6% polyetheramine, and 1% defoaming agent.

[0174] The filler includes wollastonite fiber-1 and flaky carbonyl iron powder-1 with a mass ratio of 1:0.5.

[0175] The preparation method of the fluorine-modified epoxy resin is as follows: 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane are mixed evenly, 0.5 g of tetrabutyl titanate is added, and the mixture is stirred and reacted at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0176] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:4.

[0177] The preparation method of the hot pressing magnetic powder connecting adhesive includes the following steps:

[0178] The fluorine-modified epoxy resin, the curing agent, the filler, the polyetheramine, and the defoaming agent are mixed evenly to obtain the hot pressing magnetic powder connecting adhesive.

[0179] Comparative Example 6

[0180] A hot pressing magnetic powder connecting adhesive includes the following components in weight percentage: 51% of fluorine-modified epoxy resin, 18% of curing agent, 24% of filler, 6% of polyetheramine, and 1% of defoaming agent.

[0181] The filler includes wollastonite fiber-1.

[0182] The preparation method of the fluorine-modified epoxy resin is as follows: 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane are mixed evenly, 0.5 g of tetrabutyl titanate is added, and the mixture is stirred and reacted at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0183] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0184] The preparation method of the hot pressing magnetic powder connecting adhesive includes the following steps:

[0185] The fluorine-modified epoxy resin, the curing agent, alumina, the polyetheramine, and the defoaming agent are mixed evenly to obtain the hot pressing magnetic powder connecting adhesive.

[0186] Comparative Example 7

[0187] A hot pressing magnetic powder connecting adhesive includes the following components in weight percentage: 51% of fluorine-modified epoxy resin, 18% of curing agent, 24% of filler, 6% of polyetheramine, and 1% of defoaming agent.

[0188] The filler includes flaky carbonyl iron powder-1.

[0189] The preparation method of the fluorine-modified epoxy resin is as follows: 100 g of bisphenol A epoxy resin-1 and 15 g of perfluorooctyltriethoxysilane are mixed evenly, 0.5 g of tetrabutyl titanate is added, and the mixture is stirred and reacted at 90 °C for 5 hours to obtain the fluorine-modified epoxy resin.

[0190] The curing agent includes 4,4'-diaminodiphenyl sulfone and cashew shell oil phenolic amine-1 with a mass ratio of 1:2.

[0191] The preparation method of the hot-pressing magnetic powder connecting adhesive includes the following steps:

[0192] Mix the fluorine-modified epoxy resin, curing agent, alumina, polyetheramine, and defoaming agent evenly to obtain the hot-pressing magnetic powder connecting adhesive.

[0193] Test Example

[0194] 1. Use the DSC method to test Tg and the TGA method to test Td.

[0195] 2. After placing the connecting adhesives of the examples and comparative examples at 200 °C for 1000 h respectively, test the shear strength.

[0196] Table 1

[0197]

[0198] It can be seen from Table 1 that the hot-pressing magnetic powder connecting adhesive of the present invention has extremely high Tg and Td, can work stably at 280 °C for a long time, is significantly superior to existing products (such as DM-6997), and meets the magnetic powder connection and insulation requirements in high-temperature scenarios such as oil drilling.

[0199] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A hot-pressed magnetic powder connecting adhesive, characterized in that, It comprises components in the following weight percentages: 45-65% fluorine-modified epoxy resin, 15-20% curing agent, 20-30% filler, 5-8% toughening agent, 0.5-1.5% additive; the sum of the amounts of all components is 100%; The fluorine-modified epoxy resin is obtained by reacting bisphenol A epoxy resin with perfluorooctyltriethoxysilane, and the mass ratio of bisphenol A epoxy resin to perfluorooctyltriethoxysilane is (8-5):1; The curing agent comprises 4,4'-diaminodiphenylsulfone and cashew shell oil phenolic amine with a mass ratio of 1:(0.5-2); The filler comprises wollastonite fiber and flaky carbonyl iron powder with a mass ratio of 1:(0.5-2); The viscosity of the cashew shell oil phenolic amine at 25 °C is 2300-2500 cPs, and the amine value is 340-390 mgKOH / g; The aspect ratio of the flaky carbonyl iron powder is (8-10):1; The aspect ratio of the wollastonite fiber is (12-15):1; The epoxy equivalent of the bisphenol A epoxy resin is 625-675 g / eq.

2. The hot-pressing magnetic powder connecting glue according to claim 1, characterized in that The preparation method of the fluorine-modified epoxy resin is: mixing bisphenol A epoxy resin and perfluorooctyltriethoxysilane uniformly, adding a catalyst, and reacting to obtain the fluorine-modified epoxy resin.

3. The hot-pressing magnetic powder connecting adhesive according to claim 2, wherein The catalyst is tetrabutyl titanate, and the mass ratio of bisphenol A epoxy resin to the catalyst is 100:(0.1-1).

4. The hot-pressing magnetic powder connecting adhesive according to claim 2, characterized in that The temperature of the reaction is 75-95 °C, and the reaction time is 2-8 h.

5. The hot-pressing magnetic powder connecting adhesive according to claim 1, wherein The toughening agent is polyetheramine; the additive comprises at least one of a defoaming agent and a leveling agent.

6. The preparation method of the hot-pressed magnetic powder connecting glue according to any one of claims 1 to 5, characterized in that, It comprises the following steps: Mixing the fluorine-modified epoxy resin, the curing agent, the filler, the toughening agent, and the additive uniformly to obtain the hot-pressing magnetic powder connecting adhesive.

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