Pouring sealant as well as preparation method and application thereof

Abstract

The invention relates to the technical field of pouring sealants, in particular to a pouring sealant and a preparation method and application thereof, and the pouring sealant comprises epoxy resin, a curing agent and filler; the filler comprises a first filler, a second filler and a third filler; the first filler comprises quartz and / or silica powder; the second filler comprises a flame-retardant filler; the third filler comprises fumed silica. The pouring sealant has excellent high-temperature resistance, compression performance and flame retardance after being cured, is low in flowability, can meet the application requirements of the pouring sealant for mounting the inserts for the airplane, and is particularly suitable for pouring when the inserts of the airplane are mounted at the curing temperature of 120-180 DEG C; moreover, the pouring sealant provided by the invention belongs to a single-component pouring sealant, does not need to be prepared on site when being used, and is simple to operate and convenient to use.

Description

Technical Field

[0001] The present application relates to the technical field of potting glue, and in particular to a potting glue and a preparation method and application thereof. Background Art

[0002] Epoxy resin cured products have few by-products, small shrinkage, are active to various types of curing agents, and have good bonding properties to a variety of different substrates. So far, a wide variety of product systems have been developed. Epoxy resin adhesives generally have the advantages of low cost and simple construction process, and have become an important product category in the adhesive market. Among them, potting-type epoxy resin adhesives have been widely used in machinery, electronics, aerospace, coatings and other fields. Single-component epoxy resins are simple to operate, do not require on-site preparation, and are easy to use. In recent years, they have been favored in domestic and foreign research.

[0003] CN116606619A discloses a method for preparing a one-component epoxy resin glue electronic potting glue, wherein the raw materials for preparing the one-component epoxy resin glue electronic potting glue include the following components by weight: 80-100 parts of epoxy resin, 1-3 parts of active alumina, 1-3 parts of active silicon micropowder, 0.01-0.07 parts of anti-settling agent, 0.1-0.5 parts of pigment, and 1-3 parts of curing agent. The one-component epoxy resin glue electronic potting glue disclosed herein has a long storage period at room temperature, good storage stability, strong impact resistance, and enhanced heat resistance.

[0004] CN102504494A discloses a one-component epoxy resin potting material and a preparation method thereof. The raw materials for preparing the one-component epoxy resin potting material include the following components by weight: 100 parts of epoxy resin, 73-85 parts of curing agent, 3.1-16.5 parts of isocyanate, 8.8-31.7 parts of polyether polyol, 0.3-1 part of imidazole, and 200-450 parts of filler. The one-component epoxy resin potting material disclosed herein has a heat deformation temperature of 132.1-137.1°C and an average linear expansion coefficient of 2.3×10 -5 1 / ℃, which is lower than the commonly used two-component epoxy resin potting material. It is suitable for potting electrical components with working temperature of -40℃~120℃.

[0005] CN117965119A discloses a high-performance epoxy resin adhesive and a preparation method thereof. The high-performance epoxy resin adhesive is a two-component adhesive including components A and B. Component A, by weight, includes the following components: 100 parts of epoxy resin, 10-20 parts of diluent, 10-18 parts of amino-modified inorganic material; component B, by weight, includes the following components: 100 parts of curing agent, 2-4 parts of curing accelerator, and 12-16 parts of silane coupling agent. By amino-modifying inorganic materials, not only the dispersibility of inorganic materials is improved, but also the mechanical properties of epoxy resin adhesive are enhanced.

[0006] However, the epoxy adhesives prepared by the above patents and prior art have poor mechanical properties at high temperatures and unsatisfactory flame retardant properties, and cannot meet the application requirements of aircraft insert installation potting glue.

[0007] Therefore, it is crucial to develop a potting compound that can develop the above defects. Summary of the invention

[0008] In view of the above problems, the present application provides a potting compound and a preparation method and application thereof. The potting compound has excellent high temperature resistance, compression performance and flame retardant performance after curing, and has low fluidity, which can meet the application requirements of potting compounds for aircraft insert installation, and is particularly suitable for potting during aircraft insert installation at a curing temperature in the range of 120-180°C; moreover, the potting compound described in the present application is a single-component potting compound, which does not require on-site preparation when used, and is simple to operate and easy to use.

[0009] In a first aspect, the present application provides a potting adhesive, wherein the potting adhesive comprises an epoxy resin, a curing agent and a filler;

[0010] The filler includes a first filler, a second filler and a third filler;

[0011] The first filler includes quartz and / or silicon powder;

[0012] The second filler includes a flame retardant filler;

[0013] The third filler includes fumed silica.

[0014] In the technical scheme of the implementation mode of the present application, through the coordination of the first filler, the second filler and the third filler, wherein the core function of the first filler is reinforcement, the core function of the second filler is flame retardant, and the core function of the third filler is to reduce flow by controlling the thixotropy of the system, the three work synergistically, and the cured potting glue has excellent high temperature resistance, compression performance and flame retardant performance, and low flowability, which can meet the application requirements of potting glue for aircraft insert installation, and is particularly suitable for potting during aircraft insert installation at a curing temperature in the range of 120-180°C; in addition, the potting glue described in the present application is a single-component potting glue, which does not need to be prepared on-site when used, and is simple to operate and easy to use.

[0015] In some embodiments, the mass ratio of the epoxy resin to the curing agent is 100:(30-50); and / or;

[0016] The mass ratio of the epoxy resin to the filler is 100:(20-150), and optionally 100:(40-115).

[0017] In some embodiments, the mass ratio of the first filler to the second filler is 4:(1.5-2.5); and / or;

[0018] The mass ratio of the first filler to the third filler is 4:(0.7-1.3).

[0019] In some embodiments, the particle size of the first filler is 400-1600 mesh.

[0020] In some embodiments, the mass ratio of quartz to silicon powder is 1:(0-3), optionally 1:(0.3-3).

[0021] In some embodiments, the second filler includes a metal oxide and / or a metal hydroxide.

[0022] In the technical solution of the implementation mode of the present application, the second filler is selected as a flame retardant filler in the above range because: metal oxides and metal hydroxides have good compatibility with epoxy resin and help maintain the mechanical properties of the potting glue after curing.

[0023] In some embodiments, the metal oxide includes magnesium oxide and / or aluminum oxide.

[0024] In some embodiments, the metal hydroxide includes magnesium hydroxide and / or aluminum hydroxide.

[0025] In some embodiments, the mass ratio of the metal oxide to the metal hydroxide is 1:(0.5-4).

[0026] In some embodiments, the specific surface area of ​​the third filler is 100-400m 2 / g.

[0027] In some embodiments, the epoxy value of the epoxy resin is 0.7-1.2 mol / 100g.

[0028] In some embodiments, the epoxy resin includes glycidyl ether epoxy resin and / or 4-(2,3-epoxypropoxy)-N,N-di(2,3-epoxypropyl)aniline.

[0029] In some embodiments, the glycidyl ether epoxy resin includes diphenylmethane glycidyl ether epoxy resin and / or alicyclic glycidyl ester type epoxy resin.

[0030] In some embodiments, the curing agent includes diaminodiphenyl sulfone (DDS) and / or diaminodiphenylmethane (DDM); diaminodiphenyl sulfone or a combination of diaminodiphenyl sulfone and diaminodiphenylmethane may be selected.

[0031] In the technical solution of the implementation mode of the present application, the curing agent is suitable for curing the epoxy system at high temperature, and the formed potting glue can be cured in the range of 120-180°C.

[0032] In some embodiments, the potting compound comprises the following components in parts by weight: 100 parts of epoxy resin, 30-50 parts of curing agent and 40-115 parts of filler;

[0033] The filler comprises 10-70 parts of a first filler, 5-60 parts of a second filler and 5-20 parts of a third filler.

[0034] In some embodiments, the first filler includes 10-40 parts of quartz and / or 10-30 parts of silicon powder;

[0035] The second filler comprises 5-30 parts of magnesium oxide and / or 10-30 parts of magnesium hydroxide;

[0036] The third filler includes 5-20 parts of fumed silica.

[0037] In a second aspect, the present application provides a method for preparing a potting compound, the preparation method comprising the following steps:

[0038] Mixing epoxy resin, curing agent and filler to obtain the potting glue;

[0039] The filler includes a first filler, a second filler and a third filler.

[0040] In some embodiments, before the fillers are mixed, the first filler, the second filler and the third filler are each independently dried.

[0041] In some embodiments, the mixing method includes kneading.

[0042] In some embodiments, the mixing speed is 5-20 r / min; and / or;

[0043] The mixing temperature is 20-50°C; and / or;

[0044] The mixing time is 20-30 min; and / or;

[0045] The mixing is performed under vacuum conditions.

[0046] In a third aspect, the present application provides a potting compound described in the first aspect, or a potting compound obtained by the preparation method described in the second aspect, for use in the installation of aircraft inserts.

[0047] In some embodiments, when the aircraft insert is installed, the curing temperature of the potting compound is 120-180°C.

[0048] Compared with the prior art, the technical solution of this application has the following advantages:

[0049] (1) The potting adhesive described in the present application has excellent high temperature resistance, compression performance and flame retardant performance after curing, and has low fluidity, which can meet the application requirements of potting adhesives for aircraft insert installation, and is particularly suitable for potting during aircraft insert installation at a curing temperature in the range of 120-180°C.

[0050] (2) The potting adhesive described in the present application can be cured in the range of 120-180°C; in the flowability test at 25°C, the flow length is less than 4.8 mm, and in the flowability test at 52°C, the flow length is less than 5.0 mm; the compressive strength at 25°C is more than 146 MPa, and the compressive strength at 177°C is more than 70 MPa, and can reach 85 MPa; after a 12s vertical burning test, the flame time is ≤4s, the char length is ≤94mm, and the drip flame time is ≤1s; the storage period at room temperature is more than 90 days; it can be used for potting during the installation of aircraft inserts at a curing temperature in the range of 120-180°C.

[0051] (3) The potting glue described in the present application is a single-component potting glue, which does not need to be prepared on site when used and is simple to operate and easy to use.

[0052] The above description is only an overview of the technical solution of the present application. In order to more clearly understand the technical means of the present application, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are listed below. DETAILED DESCRIPTION

[0053] The following is a detailed description of the embodiments of the technical solution of the present application. The following embodiments are only used to more clearly illustrate the technical solution of the present application, and are therefore only used as examples, and cannot be used to limit the scope of protection of the present application.

[0054] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by technicians in the technical field to which this application belongs; the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" in the description and claims of this application and any variations thereof are intended to cover non-exclusive inclusions.

[0055] In the description of the embodiments of the present application, the technical terms "first", "second", etc. are only used to distinguish different objects, and cannot be understood as indicating or implying relative importance or implicitly indicating the number, specific order or primary and secondary relationship of the indicated technical features. In the description of the embodiments of the present application, the meaning of "multiple" is more than two, unless otherwise clearly and specifically defined.

[0056] Reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present application. The appearance of the phrase in various locations in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0057] The "range" disclosed in the present application is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of the particular range. The range defined in this way can be inclusive or exclusive of the end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a range. For example, if a range of 60 to 120 and 80 to 110 is listed for a particular parameter, it is understood that a range of 60 to 110 and 80 to 120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In the present application, unless otherwise specified, the numerical range "ab" represents an abbreviation of any real number combination between a and b, where a and b are both real numbers. For example, the numerical range "2-10" means that all real numbers between "2-10" are listed in this document, and "2-10" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0058] In the description of the embodiments of the present application, the term "and / or" is only a description of the association relationship of associated objects, indicating that three relationships may exist. For example, A and / or B can represent: A exists, A and B exist at the same time, and B exists. In addition, the character " / " in this article generally indicates that the associated objects before and after are in an "or" relationship.

[0059] In the prior art, epoxy adhesives have poor mechanical properties at high temperatures and unsatisfactory flame retardancy, and are unable to meet the application requirements of aircraft insert installation potting adhesives.

[0060] The potting adhesive formed by combining different fillers in the present application has excellent high temperature resistance, compression performance and flame retardant performance after curing, and has low fluidity, which can meet the application requirements of potting adhesives for aircraft insert installation, and is particularly suitable for potting during aircraft insert installation at a curing temperature in the range of 120-180°C.

[0061] [Potting glue]

[0062] The present application provides a potting adhesive, the potting adhesive comprising epoxy resin, a curing agent and a filler;

[0063] The filler includes a first filler, a second filler and a third filler;

[0064] The first filler includes quartz and / or silicon powder;

[0065] The second filler includes a flame retardant filler;

[0066] The third filler includes fumed silica.

[0067] In the technical solution of the embodiment of the present application, through the coordination of the first filler, the second filler and the third filler, wherein the core function of the first filler is reinforcement, the core function of the second filler is flame retardant, and the core function of the third filler is to reduce flow by controlling the thixotropy of the system, the three work synergistically, and the cured potting glue has excellent high temperature resistance, compression performance and flame retardant performance, and low flowability, which can meet the application requirements of potting glue for aircraft insert installation, and is particularly suitable for potting during aircraft insert installation at a curing temperature in the range of 120-180°C; in addition, the potting glue described in the present application is a single-component potting glue, which does not need to be prepared on-site when used, and is simple to operate and easy to use.

[0068] In some embodiments, the mass ratio of the epoxy resin to the curing agent is 100:(30-50), wherein 30-50 can be 32, 34, 36, 38, 40, 42, 44, 46, 48, etc.; and / or;

[0069] The mass ratio of the epoxy resin to the filler is 100:(20-150), wherein 20-150 can be 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, etc., and can be optionally 100:(40-115).

[0070] In some embodiments, the mass ratio of the first filler to the second filler is 4:(1.5-2.5), wherein 1.5-2.5 can be 1.6, 1.8, 2, 2.2, 2.4, etc.; and / or;

[0071] The mass ratio of the first filler to the third filler is 4:(0.7-1.3), wherein 0.7-1.3 can be 1.6, 1.8, 2.0, 2.2, 2.4, etc.

[0072] In some embodiments, the particle size of the first filler is 400-1600 mesh, such as 600 mesh, 800 mesh, 1000 mesh, 1200 mesh, 1400 mesh, etc.

[0073] In this application, the particle size refers to the average particle size.

[0074] In some embodiments, the mass ratio of quartz to silicon powder is 1:(0-3), wherein 0-3 can be 0.5, 1, 1.5, 2, 2.5, etc., and can be optionally 1:(0.3-3).

[0075] In some embodiments, the second filler includes metal oxides and / or metal hydroxides.

[0076] In the technical solution of the embodiment of the present application, the second filler is selected as a flame retardant filler within the above range because: metal oxides and metal hydroxides have good compatibility with epoxy resin and help maintain the mechanical properties of the potting glue after curing.

[0077] In some embodiments, the metal oxide includes magnesium oxide and / or aluminum oxide.

[0078] In some embodiments, the metal hydroxide includes magnesium hydroxide and / or aluminum hydroxide.

[0079] In some embodiments, the mass ratio of the metal oxide to the metal hydroxide is 1:(0.5-4), wherein 0.5-4 can be 1.5, 2, 2.5, 3, 3.5, etc.

[0080] In some embodiments, the specific surface area of ​​the third filler is 100-400m 2 / g, for example 150m 2 / g, 200m 2 / g, 250m 2 / g、300m 2 / g, 350m 2 / g, etc.

[0081] In some embodiments, the epoxy value of the epoxy resin is 0.7-1.2 mol / 100g, including 0.8 mol / 100g, 0.9 mol / 100g, 1 mol / 100g, 1.1 mol / 100g, etc.

[0082] In the present application, the epoxy value refers to the amount (molar number) of substances containing epoxy groups per 100 grams of epoxy resin, with mol / 100g as the unit. The test methods for the epoxy value are hydrochloric acid pyridine method, hydrochloric acid acetone method, hydrochloric acid dioxane method, direct titration method with hydrogen bromide acetic acid solution, non-aqueous titration method with tetraethylammonium perchlorate, colorimetry, spectral analysis, etc.

[0083] In some embodiments, the epoxy resin includes glycidyl ether epoxy resin and / or 4-(2,3-epoxypropoxy)-N,N-di(2,3-epoxypropyl)aniline (AFG-90 epoxy resin).

[0084] In some embodiments, the glycidyl ether epoxy resin includes diphenylmethane glycidyl ether epoxy resin (AG-80 epoxy resin) and / or alicyclic glycidyl ester type epoxy resin (TDE-85 epoxy resin).

[0085] As an example, the information of several typical epoxy resins used in this application is as follows:

[0086] AG-80 epoxy resin is a tetrafunctional epoxy resin, also known as 4,4'-methylenebis(N,N-diglycidylaniline, with an epoxy value of 0.75-0.85 mol / 100g.

[0087] TDE-85 epoxy resin is a trifunctional alicyclic glycidyl ester epoxy resin with a unique molecular structure, containing one alicyclic epoxy group and two glycidyl ester groups, and its epoxy value is 0.85-1.00 mol / 100g.

[0088] AFG-90 epoxy resin is a trifunctional epoxy resin, its scientific name is 4-(2,3-epoxypropoxy)-N,N-di(2,3-epoxypropyl)aniline, and its epoxy value is 0.90-1.01mol / 100g.

[0089] In some embodiments, the curing agent includes diaminodiphenyl sulfone (DDS) and / or diaminodiphenylmethane (DDM); diaminodiphenyl sulfone or a combination of diaminodiphenyl sulfone and diaminodiphenylmethane may be selected.

[0090] In the technical solution of the embodiment of the present application, the curing agent is suitable for curing the epoxy system at high temperature, and the formed potting glue can be cured in the range of 120-180°C (for example, 130°C, 140°C, 150°C, 160°C, 170°C, etc.).

[0091] In some embodiments, the potting compound includes the following components in parts by weight: 100 parts of epoxy resin, 30-50 parts of curing agent and 40-115 parts of filler;

[0092] The filler comprises 10-70 parts of a first filler, 5-60 parts of a second filler and 5-20 parts of a third filler.

[0093] In some embodiments, the first filler includes 10-40 parts of quartz and / or 10-30 parts of silicon powder;

[0094] The second filler comprises 5-30 parts of magnesium oxide and / or 10-30 parts of magnesium hydroxide;

[0095] The third filler includes 5-20 parts of fumed silica.

[0096] [Preparation of potting compound]

[0097] The present application provides a method for preparing a potting compound, the preparation method comprising the following steps:

[0098] Mixing epoxy resin, curing agent and filler to obtain the potting glue;

[0099] The filler includes a first filler, a second filler and a third filler.

[0100] In some embodiments, before mixing the fillers, the first filler, the second filler and the third filler are each independently dried.

[0101] As an example, the drying temperature is 100-140°C, such as 105°C, 110°C, 115°C, 120°C, 125°C, 130°C, 135°C, etc.; and / or;

[0102] The drying time is 6-12 hours, for example, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, etc.

[0103] In some embodiments, the mixing comprises kneading.

[0104] In some embodiments, the mixing speed is 5-20 r / min; and / or;

[0105] The mixing temperature is 20-50°C; and / or;

[0106] The mixing time is 20-30 min; and / or;

[0107] The mixing is performed under vacuum conditions.

[0108] As an example, the preparation method of the potting glue includes the following steps:

[0109] (1) drying the first filler, the second filler and the third filler independently at 100-140° C. for 6-12 hours;

[0110] (2) placing the epoxy resin, curing agent and dried filler in a kneader, setting the kneader speed to 5-20 r / min and the kneading temperature to 20-50° C., evacuating the mixture and kneading in the kneader for 20-30 min, and cooling the mixture to obtain the potting glue.

[0111] [Application of potting compound]

[0112] The present application provides a potting adhesive, or a potting adhesive obtained by the preparation method, for use in the installation of aircraft inserts.

[0113] In some embodiments, when the aircraft insert is installed, the curing temperature of the potting glue is 120-180° C., such as 130° C., 140° C., 150° C., 160° C., 170° C., etc.

[0114] In practical applications, the potting glue is injected into a component that needs to be potted, such as a honeycomb panel, and cured at 120 to 180° C. (e.g., 130° C., 140° C., 150° C., 160° C., 170° C., etc.) for 0.5 to 5 h (e.g., 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, etc.) to complete the curing.

[0115] [Example]

[0116] In this application, the raw material information of each embodiment is as follows:

[0117] AG-80 epoxy resin: purchased from Shanghai Resin Factory Co., Ltd., brand name AG-80, epoxy value is 0.75-0.85 mol / 100g.

[0118] TDE-85 epoxy resin: purchased from Shanghai Resin Factory Co., Ltd., brand name TDE-85, epoxy value is 0.90-1.01 mol / 100g.

[0119] AFG-90 epoxy resin: purchased from Shanghai Resin Factory Co., Ltd., brand name AFG-90, epoxy value of 0.85-1.00 mol / 100g.

[0120] Quartz: The particle size distribution is between 400-1600 mesh.

[0121] Silica powder: particle size distribution is between 400-1600 mesh.

[0122] Fumed silica: Specific surface area is 100-400m 2 / g.

[0123] Example 1

[0124] (1) Place quartz, magnesium oxide and fumed silica in an oven at 120°C and dry for 8 hours.

[0125] (2) The raw materials were weighed into a kneader according to a weight ratio of AG-80 epoxy resin: DDS curing agent: quartz: magnesium oxide: fumed silica = 100:35:40:20:10, the kneader speed was set to 5 r / min, the kneading temperature was set to 23° C., vacuum was drawn and kneaded in the kneader for 30 min, and then cooled to room temperature to obtain the potting glue.

[0126] The method of using the potting glue is as follows: the potting glue is cured at 121° C. for 3 hours.

[0127] Example 2

[0128] (1) Place quartz, silica powder, magnesium oxide, magnesium hydroxide and fumed silica in an oven at 120°C and dry for 8 hours.

[0129] (2) The raw materials were weighed into a kneader according to the weight ratio of TDE-85 epoxy resin: DDS curing agent: quartz: silicon powder: magnesium oxide: magnesium hydroxide: fumed silica = 100:40:30:30:15:15:12, the kneader speed was set to 10 r / min, the kneading temperature was set to 23°C, the mixture was evacuated and kneaded in the kneader for 30 minutes, and then cooled to room temperature to obtain a high temperature resistant and flame retardant one-component epoxy resin potting adhesive.

[0130] The method of using the potting glue is as follows: the potting glue is first cured at 121° C. for 1 hour, and then cured at 177° C. for 0.5 hour to complete the curing.

[0131] Example 3

[0132] (1) Place quartz, silicon powder, magnesium hydroxide and fumed silica in an oven at 120°C and dry for 8 hours.

[0133] (2) The raw materials were weighed into a kneader according to the weight ratio of AFG-90 epoxy resin: DDS curing agent: quartz: silicon powder: magnesium hydroxide: fumed silica = 100:40:20:20:25:12, the kneader speed was set to 5 r / min, the kneading temperature was set to 23° C., the mixture was evacuated and kneaded in the kneader for 20 min, and then cooled to room temperature to obtain a high temperature resistant and flame retardant one-component epoxy resin potting adhesive.

[0134] The method for using the potting glue is as follows: the potting glue is cured at 150° C. for 2 hours.

[0135] Example 4

[0136] (1) Place quartz, silicon powder, magnesium oxide, magnesium hydroxide and fumed silica in an oven at 120°C and dry for 8 hours.

[0137] (2) The raw materials were weighed into a kneader according to the weight ratio of TDE-85 epoxy resin: DDS curing agent: quartz: silicon powder: magnesium oxide: magnesium hydroxide: fumed silica = 100:40:20:20:14:12:10, the kneader speed was set to 10 r / min, the kneading temperature was set to 23°C, the mixture was evacuated and kneaded in the kneader for 30 minutes, and then cooled to room temperature to obtain a high temperature resistant and flame retardant one-component epoxy resin potting adhesive.

[0138] (3) The method of using the potting glue is as follows: the potting glue is first cured at 121° C. for 1 hour, and then cured at 177° C. for 0.5 hour to complete the curing.

[0139] Example 5

[0140] The difference between this embodiment and embodiment 1 is that magnesium oxide is replaced by hollow glass microspheres of equal mass, and the rest is the same as embodiment 1.

[0141] Example 6

[0142] The difference between this embodiment and embodiment 1 is that the mass ratio of quartz to fumed silica is 4:0.5, specifically, AG-80 epoxy resin: DDS curing agent: quartz: magnesium oxide: fumed silica = 100:35:44.5:20:5.5, and the rest is the same as embodiment 1.

[0143] Example 7

[0144] The difference between this embodiment and embodiment 1 is that the mass ratio of quartz to fumed silica is 4:1.5, specifically, AG-80 epoxy resin: DDS curing agent: quartz: magnesium oxide: fumed silica = 100:35:36:20:14, and the rest is the same as embodiment 1.

[0145] Comparative Example 1

[0146] The difference between this comparative example and Example 1 is that 40 parts of quartz are replaced by 27 parts and 13 parts of magnesium oxide and fumed silica, AG-80 epoxy resin: DDS curing agent: magnesium oxide: fumed silica = 100:35:47:23, and the rest are the same as Example 1.

[0147] Comparative Example 2

[0148] The difference between this comparative example and Example 1 is that 20 parts of magnesium oxide powder are replaced by 16 parts of quartz and 4 parts of fumed silica, AG-80 epoxy resin: DDS curing agent: quartz: fumed silica = 100:35:56:14, and the rest are the same as Example 1.

[0149] Comparative Example 3

[0150] The difference between this comparative example and Example 1 is that 10 parts of fumed silica are replaced by 7 parts of quartz and 3 parts of magnesium oxide, AG-80 epoxy resin: DDS curing agent: quartz: magnesium oxide = 100:35:47:23, and the rest are the same as Example 1.

[0151] Comparative Example 4

[0152] The difference between this comparative example and Example 1 is that quartz is replaced by zinc oxide of equal mass, and the rest is the same as Example 1.

[0153] [Performance test]

[0154] After the fully cured sealant is stored at room temperature for 90 days, it is tested according to the MAS6641B standard. The test items include density, fluidity, compression performance and flame retardancy.

[0155] The test results are summarized in Table 1.

[0156] Table 1

[0157]

[0158] Analysis of the data in Table 1 shows that the potting glue described in the present application can be cured in the range of 120-180°C; in the flowability test at 25°C, the flow length is less than 4.8mm, and in the flowability test at 52°C, the flow length is less than 5.0mm; the compressive strength at 25°C is above 146MPa, and the compressive strength at 177°C is above 70MPa, and can reach 85MPa; after a 12s vertical burning test, the flame time is ≤4s, the charred length is ≤94mm, and the drip flame time is ≤1s; the storage period at room temperature is more than 90 days; it can be used for potting during the installation of aircraft inserts at a curing temperature in the range of 120-180°C.

[0159] Analysis of comparative examples 1-3 and embodiment 1 shows that the performance of comparative examples 1-3 is not as good as that of embodiment 1, which proves that the potting glue formed by the combination of the first filler, the second filler and the third filler has better performance.

[0160] Analysis of Comparative Example 4 and Example 1 shows that the performance of Comparative Example 4 is not as good as that of Example 1, which proves that the potting glue formed by the first filler within the range described in the present application has better performance.

[0161] Analysis of Example 5 and Example 1 shows that the performance of Example 5 is not as good as that of Example 1, which proves that the potting glue formed by the second filler within the range described in the present application has better performance.

[0162] Analysis of Examples 6-7 and Example 1 shows that the performance of Examples 6-7 is not as good as that of Example 1, which proves that the potting glue formed by the mass ratio of the first filler, the second filler and the third filler within the said range has better performance.

[0163] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them; although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application, and they should all be included in the scope of the claims and specification of the present application. In particular, as long as there is no structural conflict, the various technical features mentioned in the various embodiments can be combined in any way. The present application is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.

Claims

1. A potting glue, characterized in that: The potting glue comprises epoxy resin, curing agent and filler; The filler includes a first filler, a second filler and a third filler; The first filler includes quartz and / or silicon powder; The second filler includes a flame retardant filler; The third filler includes fumed silica.

2. The potting compound according to claim 1, characterized in that: The mass ratio of the epoxy resin to the curing agent is 100:(30-50); and / or; The mass ratio of the epoxy resin to the filler is 100:(20-150), and optionally 100:(40-115).

3. The potting glue according to claim 1 or 2, characterized in that: The mass ratio of the first filler to the second filler is 4:(1.5-2.5); and / or; The mass ratio of the first filler to the third filler is 4:(0.7-1.3).

4. The potting adhesive according to any one of claims 1 to 3, characterized in that: The particle size of the first filler is 400-1600 mesh; Preferably, the mass ratio of quartz to silicon powder is 1:(0-3), optionally 1:(0.3-3).

5. The potting adhesive according to any one of claims 1 to 4, characterized in that: The second filler comprises metal oxide and / or metal hydroxide; Preferably, the metal oxide comprises magnesium oxide and / or aluminum oxide; Preferably, the metal hydroxide comprises magnesium hydroxide and / or aluminum hydroxide; Preferably, the mass ratio of the metal oxide to the metal hydroxide is 1:(0.5-4).

6. The potting adhesive according to any one of claims 1 to 5, characterized in that: The specific surface area of ​​the third filler is 100-400m 2 / g.

7. The potting adhesive according to any one of claims 1 to 6, characterized in that: The epoxy value of the epoxy resin is 0.7-1.2 mol / 100g; Preferably, the epoxy resin comprises glycidyl ether epoxy resin and / or 4-(2,3-epoxypropoxy)-N,N-di(2,3-epoxypropyl)aniline; Preferably, the glycidyl ether epoxy resin comprises diphenylmethane glycidyl ether epoxy resin and / or alicyclic glycidyl ester type epoxy resin; The curing agent includes diaminodiphenyl sulfone and / or diaminodiphenylmethane; diaminodiphenyl sulfone or a combination of diaminodiphenyl sulfone and diaminodiphenylmethane can be selected.

8. The potting adhesive according to any one of claims 1 to 7, characterized in that: The potting glue comprises the following components in parts by weight: 100 parts of epoxy resin, 30-50 parts of curing agent and 40-115 parts of filler; The filler comprises 10-70 parts of a first filler, 5-60 parts of a second filler and 5-20 parts of a third filler; Preferably, the first filler comprises 10-40 parts of quartz and / or 10-30 parts of silicon powder; The second filler comprises 5-30 parts of magnesium oxide and / or 10-30 parts of magnesium hydroxide; The third filler includes 5-20 parts of fumed silica.

9. A method for preparing a potting compound, characterized in that: The preparation method comprises the following steps: Mixing epoxy resin, curing agent and filler to obtain the potting glue; The filler includes a first filler, a second filler and a third filler; Preferably, before mixing the fillers, the first filler, the second filler and the third filler are dried independently; Preferably, the mixing method includes kneading; Preferably, the mixing speed is 5-20 r / min; and / or; The mixing temperature is 20-50°C; and / or; The mixing time is 20-30 min; and / or; The mixing is performed under vacuum conditions.

10. Use of the potting adhesive according to any one of claims 1 to 8, or the potting adhesive obtained by the preparation method according to claim 9, in the installation of aircraft inserts; Preferably, when the aircraft insert is installed, the curing temperature of the potting glue is 120-180°C.

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