High flame-retardant potting adhesive and preparation method thereof

Abstract

The application discloses high-flame-retardant pouring sealant and a preparation method thereof, and belongs to the field of flame-retardant materials. The pouring sealant comprises component A and component B. The component A comprises the following raw materials: base glue, inorganic filler, titanium white, flame retardant and deep curing agent. The component B comprises the following raw materials: diluent, waterproof agent, crosslinking agent, coupling agent and catalyst. The inorganic filler comprises at least one of aluminum hydroxide or magnesium hydroxide, and the flame retardant comprises at least one of UN-333, melamine phosphate, melamine cyanurate or melamine polyphosphate. The high-flame-retardant pouring sealant can improve the flame retardance of the product by adding a small amount of flame retardant, and can also add a proper amount of magnesium hydroxide filler to enhance the flame retardance, and the flame retardance grade is UL94 V0. The pouring sealant can realize deep curing quickly, has the synchronous curing effect of the colloid surface and the inside, and simultaneously has excellent tensile strength, elongation at break, low glue viscosity, good fluidity and excellent aging resistance.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of flame-retardant materials, in particular to a high flame-retardant pouring sealant and a preparation method thereof. BACKGROUND

[0002] Pouring seal refers to pouring liquid composite material into a device containing electronic components and circuit by mechanical or manual method, and curing into a thermosetting polymer insulating material with excellent performance under normal temperature or heating condition; it can strengthen the integrity of electronic device, improve the resistance of device to external impact and vibration; it is conducive to miniaturization and light weight of device; it can avoid direct exposure of components and circuit, improve the waterproof and moisture-proof performance of device, and improve the use performance and stability parameters.

[0003] The pouring sealant for junction box of photovoltaic module can seal and bond the battery pieces, circuit boards and other equipment inside the module, and plays an important role in improving the quality of junction box and protecting internal components from external environment. The photovoltaic module is exposed to the external environment for a long time, and is inevitably affected by high temperature, rain, dust and other factors. When the internal electronic components are overloaded or short-circuited and catch fire, it is very important to use high flame-retardant pouring sealant to ensure the long-term stable operation of electronic module.

[0004] Patent CN107474789A discloses a kind of two-component pouring sealant A agent masterbatch, two-component pouring sealant and preparation method thereof, the masterbatch is mainly prepared from the following components by weight: 1-2 weight parts of base glue, 4-5 weight parts of aluminum hydroxide, 0.05-0.06 weight parts of titanium white and 0.04-0.05 weight parts of stearic acid, the B agent is mainly composed of the following components by weight: tetraethyl orthosilicate 0.5-1.5 weight parts, polyether 1-2 weight parts, methyl trimethoxysilane 0.7-0.8 weight parts, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane 0.2-0.3 weight parts, glycidyl ether oxypropyl trimethoxysilane 0.05-0.1 weight parts, dibutyltin dilaurate 0.005-0.006 weight parts; the viscosity of A agent is low, the stability is better, and when mixed with B agent, the mixed viscosity is low, the leveling property is better, the bubbles are easy to discharge, and the mechanical properties of the two-component pouring sealant prepared therefrom are improved, the wrinkles and cracks of the two-component pouring sealant after curing are improved, so that the performance of the pouring sealant is more superior in storage, use and protection, and the comprehensive performance is greatly improved. However, it does not indicate the changes of tensile strength, elongation at break, adhesion properties and aging performance of the pouring sealant. SUMMARY

[0005] In order to solve the technical problems of the prior art, the main purpose of the present application is to provide a high flame-retardant pouring sealant and a preparation method thereof.The pouring sealant has excellent tensile strength, elongation at break, adhesion properties, aging performance and flame-retardant performance, and has moderate viscosity and good flowability.

[0006] In order to achieve the above-mentioned purpose, the technical scheme adopted by the present application is:

[0007] A high flame-retardant pouring sealant, the pouring sealant comprises A component and B component,

[0008] The A component comprises the following raw materials in parts by weight: base glue 300-320 parts, inorganic filler 230-250 parts, titanium white 10-20 parts, flame retardant 30-0 parts, deep curing agent 1-5 parts;

[0009] The B component comprises the following raw materials in parts by weight: diluent 50-60 parts, waterproof agent 25-35 parts, crosslinking agent 5-10 parts, coupling agent 5-10 parts, catalyst 0.1-1 part.

[0010] Preferably, the mass ratio of the A component to the B component is 3-8:1.

[0011] More preferably, the mass ratio of the A component to the B component is 6:1.

[0012] Preferably, the base glue is 107 silicone rubber, and the viscosity is 1000-2000 mPa·s.

[0013] More preferably, the viscosity of the base glue is 1500 mPa·s.

[0014] Preferably, the inorganic filler is selected from at least one of aluminum hydroxide or magnesium hydroxide.

[0015] Preferably, the flame retardant is selected from at least one of UN-333, melamine phosphate, melamine cyanurate or melamine polyphosphate.

[0016] Preferably, the diluent is dimethyl silicone oil, and the viscosity is 100 mPa·s.

[0017] Preferably, the waterproof agent is polymethyl triethoxysilane;

[0018] The crosslinking agent is selected from at least one of ethyl orthosilicate, polyethyl silicate or dimethyl diethoxysilane;

[0019] More preferably, the crosslinking agent is ethyl orthosilicate.

[0020] The coupling agent is selected from at least one of gamma-aminopropyl triethoxysilane or N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane;

[0021] The catalyst is selected from at least one of di-n-butyl tin dilaurate, stannous octoate or triethyl tin diamine.

[0022] More preferably, the catalyst is di-n-butyl tin dilaurate.

[0023] The application also provides a preparation method of the high flame-retardant pouring sealant, comprising the following steps:

[0024] S1, mixing the base glue, inorganic filler, titanium white and flame retardant under normal pressure by mechanical stirring, and then stirring and mixing uniformly under vacuum condition by planetary machine;

[0025] S2, adding deep curing agent to the mixture, stirring and mixing uniformly under normal pressure by planetary machine, and then stirring and mixing under vacuum condition, and discharging to obtain component A;

[0026] S3, preparation of component B: mixing diluent, waterproof agent, coupling agent, crosslinking agent and catalyst in a fluorinated bottle to obtain component B;

[0027] S4, mixing and curing: mixing components A and B to obtain the flame-retardant pouring sealant.

[0028] Preferably, in the step S1, the vacuum degree of the vacuum condition is -0.1~ -0.09 MPa.

[0029] The mechanical stirring speed is 2000~2200 r / min, and the stirring time is 30~40 min.

[0030] The planetary machine stirring speed is 150~170 r / min, and the stirring time is 5~10 min.

[0031] Preferably, in the step S2, the planetary machine stirring speed is 150~170 r / min, and the stirring time is 30~40 min.

[0032] The vacuum degree of the vacuum condition is -0.1~ -0.09 MPa, and the stirring time is 5~10 min.

[0033] Compared with the prior art, the application has the following beneficial effects:

[0034] 1. The application uses low-viscosity 107 glue as the main crosslinking raw material, adds inorganic filler and flame retardant to improve the flame-retardant effect, dilutes component B into different viscosities by using diluent, crosslinks component A into a network structure by using crosslinking agent, makes the system form adhesion by using coupling agent, catalyzes the whole crosslinking system by using catalyst, and makes the crosslinking system have waterproof property by using waterproof agent. At the same time, the low viscosity of 107 glue makes component A and component B have excellent flow-out, flow-flat property and low mixing viscosity during the mixing process, greatly improves the operable time, and can ensure that the bubbles are discharged in time and the appearance is flat.

[0035] 2. The potting glue improves the flame retardance of the product by adding a small amount of flame retardant, and the flame retardance grade reaches UL94 V0 level; the tensile strength and elongation at break after DH1000 aging can be maintained above 75%; and deep curing can be quickly realized, and the surface and internal synchronous curing effect of the glue body is realized.

[0036] 3. The components of the application are matched to make the flame-retardant potting glue have good comprehensive performance, and the preparation method is simple and easy to realize, and is suitable for industrial production. DETAILED DESCRIPTION

[0037] The deep curing agent in the following examples is M-1320 deep curing agent, and UN-333 is purchased from Shanghai You Nai Organic Silicon Material Co., Ltd.

[0038] Example 1:

[0039] A high flame-retardant potting glue comprises A component and B component:

[0040] The A component comprises the following raw materials by weight: 107 glue (viscosity 1500 mPa·s) 300 parts, aluminum hydroxide 240 parts, titanium white (vanadium titanium) 15 parts, UN-333 30 parts, melamine phosphate 15 parts, and deep curing agent 3 parts;

[0041] The B component comprises the following raw materials by weight: dimethyl silicone oil (viscosity 100 mPa·s) 55 parts, polymethyl triethoxysilane 29 parts, ethyl silicate 8 parts, 3.9 parts of γ-aminopropyl triethoxysilane, 3.5 parts of N-β-(aminoethyl)-γ-aminopropyl trimethoxysilane, and dibutyltin dilaurate 0.6 parts;

[0042] The preparation method of the high flame-retardant potting glue comprises the following steps:

[0043] S1, 107 glue, aluminum hydroxide, titanium white, UN-333 and melamine phosphate are mixed under normal pressure at a mechanical stirring speed of 2100 r / min for 30 min, and then planetary stirring is carried out under a vacuum degree of-0.095 MPa for 5 min;

[0044] S2, the deep curing agent is added to the mixture obtained in step S1, and planetary stirring is carried out at a stirring speed of 160 r / min under normal pressure for 30 min, and then planetary stirring is carried out under a vacuum degree of-0.095 MPa for 5 min, to obtain the A component;

[0045] S3, the dimethyl silicone oil, polymethyl triethoxysilane, tetraethyl orthosilicate, gamma-aminopropyl triethoxysilane, N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane and dibutyl tin dilaurate are mixed uniformly in a fluorinated bottle, and a component B is obtained;

[0046] S4, the component A and the component B are mixed uniformly according to a mass ratio of 6:1, and a high flame-retardant pouring sealant with low viscosity and synchronous internal curing of the colloid is obtained.

[0047] Example 2:

[0048] A high flame-retardant pouring sealant comprises a component A and a component B.

[0049] The component A comprises the following raw materials in parts by weight: 107 glue (viscosity 1500 mPa·s) 300 parts, aluminum hydroxide 180 parts, magnesium hydroxide 60 parts, titanium white (vanadium titanium) 15 parts, UN-333 30 parts, melamine phosphate 15 parts, and deep curing agent 3 parts.

[0050] The component B comprises the following raw materials in parts by weight: dimethyl silicone oil (viscosity 100 mPa·s) 55 parts, polymethyl triethoxysilane 29 parts, tetraethyl orthosilicate 8 parts, gamma-aminopropyl triethoxysilane 3.9 parts, N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane 3.5 parts, and dibutyl tin dilaurate 0.6 parts.

[0051] The preparation method of the high flame-retardant pouring sealant comprises the following steps:

[0052] S1, 107 glue, aluminum hydroxide, titanium white, UN-333 30 parts, melamine phosphate 15 parts are mixed under normal pressure at a mechanical stirring speed of 2100 r / min for 30 min, and then planetary stirring is carried out under vacuum condition of-0.095 MPa for 5 min;

[0053] S2, the deep curing agent is added to the mixture obtained in step S1, and planetary stirring is carried out under normal pressure at a stirring speed of 160 r / min for 30 min, and then planetary stirring is carried out under vacuum condition of-0.095 MPa for 5 min, and a component A is obtained.

[0054] S3, the dimethyl silicone oil, polymethyl triethoxysilane, tetraethyl orthosilicate, gamma-aminopropyl triethoxysilane, N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane and dibutyl tin dilaurate are mixed uniformly in a fluorinated bottle, and a component B is obtained.

[0055] S4, the component A and the component B are mixed uniformly according to a mass ratio of 6:1, and a high flame-retardant pouring sealant with low viscosity and synchronous internal curing of the colloid is obtained.

[0056] Embodiment 3

[0057] A high flame-retardant pouring sealant comprises an A component and a B component:

[0058] The A component comprises the following raw materials by weight: 107 glue (viscosity 1500 mPa·s) 315 parts, aluminum hydroxide 192 parts, 48 parts of magnesium hydroxide, titanium white powder (vanadium titanium) 15 parts, UN-333 20 parts, melamine phosphate 10 parts, deep curing agent 3 parts;

[0059] The B component comprises the following raw materials by weight: dimethyl silicone oil (viscosity 100 mPa·s) 55 parts, polymethyl triethoxysilane 29 parts, ethyl orthosilicate 8 parts, 3.9 parts of γ-aminopropyl triethoxysilane, 3.5 parts of N-β-(aminoethyl)-γ-aminopropyl trimethoxysilane, dibutyl tin dilaurylate 0.6 parts;

[0060] The preparation method of the high flame-retardant pouring sealant comprises the following steps:

[0061] S1, mix 107 glue, aluminum hydroxide and titanium white powder under normal pressure at a mechanical stirring speed of 2100 r / min for 30 min, and then stir and mix in a planetary machine under a vacuum degree of-0.095 MPa for 5 min;

[0062] S2, add deep curing agent to the mixture obtained in step S1, and stir and mix in a planetary machine under normal pressure at a stirring speed of 160 r / min for 30 min, and then continue to stir and mix under a vacuum degree of-0.095 MPa for 5 min, namely the A component;

[0063] S3, mix dimethyl silicone oil, polymethyl triethoxysilane, ethyl orthosilicate, γ-aminopropyl triethoxysilane, N-β-(aminoethyl)-γ-aminopropyl trimethoxysilane and dibutyl tin dilaurylate in a fluorinated bottle to mix uniformly, namely the B component;

[0064] S4, mix the A component and the B component uniformly according to a mass ratio of 6:1 to obtain a high flame-retardant pouring sealant with low viscosity and synchronous curing inside the glue body.

[0065] Embodiment 4

[0066] A high flame-retardant pouring sealant comprises an A component and a B component:

[0067] The A component comprises the following raw materials by weight: 107 glue (viscosity 1500 mPa·s) 315 parts, aluminum hydroxide 160 parts, 80 parts of magnesium hydroxide, titanium white powder (vanadium titanium) 15 parts, UN-333 20 parts, melamine phosphate 10 parts, deep curing agent 3 parts;

[0068] The B component comprises the following raw materials by weight: dimethyl silicone oil (viscosity 100 mpa.s) 55 parts, polymethyl triethoxysilane 29 parts, ethyl orthosilicate 8 parts, 3.9 parts of gamma-aminopropyl triethoxysilane, 3.5 parts of N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane, dibutyl tin dilaurate 0.6 parts;

[0069] The preparation method of the high-flame-retardant pouring sealant comprises the following steps:

[0070] S1, 107 glue, aluminum hydroxide, titanium dioxide, under normal pressure, the mechanical stirring speed is 2100 r / min, and the mixing time is 30 min. After uniform dispersion, the planetary mixer is stirred and mixed under the vacuum condition of-0.095 MPa for 5 min;

[0071] S2, add the deep curing agent to the mixture obtained in S1, and stir and mix at a stirring speed of 160 r / min under normal pressure for 30 min, and then continue to stir and mix under the vacuum condition of-0.095 MPa for 5 min, namely the A component;

[0072] S3, shake and mix dimethyl silicone oil, polymethyl triethoxysilane, ethyl orthosilicate, gamma-aminopropyl triethoxysilane, N-beta-(aminoethyl)-gamma-aminopropyl trimethoxysilane and dibutyl tin dilaurate in a fluorinated bottle, namely the B component;

[0073] S4, mix the A component and the B component uniformly according to the mass ratio of 6:1 to obtain a high-flame-retardant pouring sealant with low viscosity and synchronous curing inside the glue body.

[0074] Comparative Example 1:

[0075] The same as Example 1, the only difference is that the melamine phosphate is replaced by melamine polyphosphate.

[0076] Comparative Example 2:

[0077] The same as Example 1, the only difference is that the melamine phosphate is replaced by melamine cyanurate.

[0078] Comparative Example 3:

[0079] The same as Example 1, the only difference is that the aluminum hydroxide is 275 parts, and UN-333 and melamine phosphate are not contained.

[0080] Comparative Example 4:

[0081] The same as Example 3, the only difference is that the melamine phosphate is replaced by melamine cyanurate.

[0082] Comparative Example 5:

[0083] The same as example 3, the only difference is that the flame retardant is 10 parts of UN-333 and 5 parts of melamine phosphate.

[0084] The mixed viscosity, tensile strength, elongation at break, flame retardant performance (characterized by its burning time) and mechanical properties after DH1000 aging of the potting sealant prepared in examples 1-4 and comparative examples 1-5 are determined, and the results are shown in table 1.

[0085] Table 1

[0086]

[0087] According to table 1, it can be seen from examples 1-4 and comparative examples 1-5 that the addition of flame retardant can reduce the viscosity and tensile strength of the potting sealant, and the mutual use of flame retardants UN-333, melamine phosphate and cyanuric acid melamine has obvious effect on improving the flame retardant performance of the potting sealant, and the flame retardant effect of melamine polyphosphate is general; it can be seen from examples 2-3 that increasing the content of flame retardant can improve the flame retardant performance of the potting sealant.

[0088] It can be seen from examples 1-4 that magnesium hydroxide can improve the viscosity and tensile strength of the potting sealant, and can greatly improve the flame retardant properties of the potting sealant, the mechanical properties of the potting sealant after DH1000 aging are good, and the aging resistance of magnesium hydroxide is better than that of aluminum hydroxide.

[0089] The potting sealant prepared by the application has excellent tensile strength, elongation at break, low adhesive viscosity, good flowability and excellent aging resistance, and the flame retardant grade can easily reach UL94V0 level.

[0090] The above examples are only preferred technical solutions of the application, and should not be regarded as limiting the application, the protection scope of the application should be the technical solutions recited in the claims, including the equivalent replacement solutions of the technical features recited in the claims as the protection scope. That is, equivalent replacement improvements within this scope are also within the protection scope of the application.

Claims

1. A high flame-retardant potting compound, characterized in that, The potting compound comprises component A and component B. Component A comprises the following raw materials in parts by weight: 300-320 parts base rubber, 230-250 parts inorganic filler, 10-20 parts titanium dioxide, 30-50 parts flame retardant, and 1-5 parts deep curing agent; wherein the base rubber is 107 silicone rubber with a viscosity of 1000-2000 mPa·s; the flame retardant is composed of UN-333 and melamine phosphate; and the deep curing agent is M-1320 deep curing agent. Component B comprises the following raw materials in parts by weight: 50-60 parts diluent, 25-35 parts waterproofing agent, 5-10 parts crosslinking agent, 5-10 parts coupling agent, and 0.1-1 parts catalyst.

2. The high flame-retardant potting compound according to claim 1, characterized in that, The mass ratio of component A to component B is 3-8:

1.

3. The high flame-retardant potting compound according to claim 1, characterized in that, The inorganic filler is selected from at least one of aluminum hydroxide or magnesium hydroxide.

4. The high flame-retardant potting compound according to claim 1, characterized in that, The diluent is dimethyl silicone oil with a viscosity of 100 mPa·s.

5. The high flame-retardant potting compound according to claim 1, characterized in that, The waterproofing agent is polymethyltriethoxysilane; The crosslinking agent is selected from at least one of tetraethyl orthosilicate, polyethyl orthosilicate, or dimethyldiethoxysilane. The coupling agent is selected from at least one of γ-aminopropyltriethoxysilane or N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane; The catalyst is selected from at least one of di-n-butyltin dilaurate, stannous octoate, or triethylenetin diamine.

6. A method for preparing the high flame-retardant potting compound according to any one of claims 1-5, characterized in that, S1. After mechanically mixing the base adhesive, inorganic filler, titanium dioxide and flame retardant under normal pressure, the mixture is then stirred and mixed evenly under vacuum conditions using a planetary mixer. S2. Add a deep curing agent to the above mixture, stir and mix evenly with a planetary mixer under normal pressure, then stir and mix under vacuum conditions to obtain component A. Preparation of S3 and B components: Mix the diluent, waterproofing agent, coupling agent, crosslinking agent and catalyst evenly in a fluorinated bottle to obtain component B; S4. Mixing and curing: Mix components A and B to obtain the high flame retardant potting compound.

7. The method for preparing the high flame-retardant potting compound according to claim 6, characterized in that, In step S1, the vacuum level is -0.1 to -0.09 MPa. The mechanical stirring speed is 2000~2200 r / min, and the stirring time is 30~40 min; The planetary mixer has a stirring speed of 150~170 r / min and a stirring time of 5~10 min.

8. The method for preparing the high flame-retardant potting compound according to claim 6, characterized in that, In step S2, the planetary mixer stirring speed is 150~170 r / min, and the stirring time is 30~40 min; The vacuum level is -0.1 to -0.09 MPa; the stirring time is 5 to 10 minutes.

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