A two-component silane-modified polyether type three-proof adhesive and its preparation method

Abstract

The present invention discloses a two-component silane-modified polyether-type three-proof adhesive and its preparation method. It includes component A and component B. Component A is composed of the following substances in parts by weight: 50-70 parts of a silane-terminated polyurethane resin, 1-5 parts of a silane coupling agent, 1-8 parts of a curing agent, 0.1-0.5 parts of an antioxidant, 0.5-1 parts of a water scavenger, 10-30 parts of a plasticizer, and 10-20 parts of a flame-retardant filler A; and component B is composed of the following substances in parts by weight: 40-60 parts of an epoxy resin, 20-40 parts of a plasticizer, 1-2 parts of distilled water, 0.1-0.5 parts of a catalyst, and 10-20 parts of a flame-retardant filler B. The two-component silane-modified polyether-type three-proof adhesive synthesized by the present invention compensates for the poor adhesion and hard film-forming shortcomings of existing different types of three-proof paints. It does not contain isocyanate groups, is solvent-free, has low viscosity, and is suitable for brushing and spraying.

Description

Technical Field

[0001] The invention belongs to the technical field of electronic circuit board coating materials, and particularly relates to a two-component silane-modified polyether type three-proof adhesive and a preparation method thereof. Background Art

[0002] With the advancement of technology, automotive controls, consumer electronics, and smart home appliances are constantly being upgraded. The safety and stability of electronic and electrical equipment are crucial. Electronic circuit boards typically require a 40-60μm thick coating. After curing, it forms a transparent or translucent protective film on the surface, providing waterproofing, insulation, salt spray resistance, mildew resistance, and corrosion resistance. This type of coating is commonly referred to as conformal coating or paint. Based on the resin type, it is generally categorized as acrylate, polyurethane, and silicone. Based on the solvent type, it can be categorized as solvent-free, water-based, or bulk. Polyurethanes offer a wide range of performance adjustments, but the terminal free reactive groups are isocyanate (-NCO), which is harmful to human contact. Water-based polyurethanes meet environmental standards and work by drying out after application. However, residual traces of water can degrade the performance of electronic devices. Acrylates are typically solution-based, with a high solvent content, posing a health risk to workers and the environment. Currently, silicone three-proof adhesive is widely used. The bond energy of silicone structure is low, and it has little impact on the working process of electronic components. The disadvantage is that the bonding strength to the substrate is weak, and the bonding damage at the interface can easily cause the sealing effect to deteriorate during long-term use.

[0003] Patent CN111393966A provides a solvent-free, silane-modified polyether conformal coating with good adhesion to substrates, high tensile strength, and excellent flexibility. It also possesses excellent water and salt spray resistance. However, the single-component sizing is convenient to apply and has a short surface drying time. However, because it cures layer by layer upon exposure to moisture, it takes a long time to fully cure, and the curing time can be extended several times in winter. Patent CN201911065005.1 discloses a polyurethane-acrylic conformal coating that does not contain organic solvents and solves the problem of difficult curing in dark areas through UV-moisture dual curing. It has excellent hardness, flexibility, water resistance, and acid and alkali resistance. However, because moisture curing retains the isocyanate group at one end of the molecular chain, long-term exposure poses potential health hazards. Summary of the Invention

[0004] The object of the present invention is to provide a two-component silane-modified polyether type three-proof adhesive and a preparation method thereof.

[0005] A two-component silane-modified polyether-type conformal adhesive, comprising component A and component B, wherein component A is composed of the following substances in parts by weight: 50-70 parts of a silane-terminated polyurethane resin, 1-5 parts of a silane coupling agent, 1-8 parts of a curing agent, 0.1-0.5 parts of an antioxidant, 0.5-1 parts of a water scavenger, 10-30 parts of a plasticizer, and 10-20 parts of a flame retardant filler A;

[0006] The B component is composed of the following materials in parts by weight: 40-60 parts of epoxy resin, 20-40 parts of plasticizer, 1-2 parts of distilled water, 0.1-0.5 parts of catalyst, and 10-20 parts of flame retardant filler B;

[0007] The weight ratio of component A to component B is (2.5-5):1.

[0008] The silane-terminated polyurethane resin is Wacker brand STP-E35, STP-E15 terminal silane-based polyurethane resin; Zhongyuan Chemical's SAX400 and SAX750 terminal silane-based polyurethane resins; Zhejiang Huangma Technology's brand 12 terminal silane-based polyurethane resin; Ruiyang Antai's brand 30 terminal silane-based polyurethane resin.

[0009] The silane coupling agent is one or more of KH-540, KH-550, KH-560, KH-570, A-1120, and A-1146.

[0010] The curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0011] The antioxidant is one or more of antioxidants 1010, 245, and BHT; the dehydrating agent is one or more of calcium oxide, xylene, and dehydrating agent A-171; and the plasticizer is diisodecyl phthalate and / or diisononyl phthalate.

[0012] The flame retardant filler A is aluminum hydroxide or aluminum oxide.

[0013] The catalyst is titanate.

[0014] The flame retardant filler B is phosphite and / or polyphosphate.

[0015] The preparation method of the A component is as follows: end-silyl polyurethane resin, silane coupling agent, antioxidant, flame retardant filler A, and plasticizer are added into a reaction kettle according to parts by weight, the temperature is raised to 110-120° C., the vacuum degree is not less than -0.095 MPa, dehydration is performed for 1-2 hours, the temperature is lowered to below 45° C., a dehydrating agent and a curing agent are added, the mixture is stirred for 20-40 minutes, and then sealed and packaged.

[0016] The preparation method of the B component is as follows: epoxy resin, plasticizer, distilled water, flame retardant filler B, and catalyst are sequentially added into a reactor according to parts by weight, fully stirred for 0.5-2 hours, and after the moisture content is tested to be within the range of 1000-5000ppm, the material is discharged and packaged.

[0017] The beneficial effects of the present invention are as follows: the two-component silane-modified polyether-type conformal adhesive synthesized by the present invention makes up for the shortcomings of poor adhesion and hard film formation of existing different types of conformal coatings. The end-silane-modified polyether is selected as the base resin, and is compounded with epoxy resin, silane coupling agent, curing agent, flame retardant filler A, flame retardant filler B and other types of additives. It does not contain isocyanate groups, is solvent-free, has low viscosity, and is suitable for brushing and spraying. DETAILED DESCRIPTION

[0018] To facilitate understanding of the present invention, the present invention will be described more fully below. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0019] Example 1

[0020] A two-component silane-modified polyether type three-proof adhesive, comprising component A and component B, wherein component A is composed of the following materials in parts by weight: 60 parts of terminal silane-based polyurethane resin (Wacker brand STP-E35), silane coupling agent KH-540 4 parts, curing agent 6 parts, antioxidant 10100.3 parts, calcium oxide 0.8 parts, diisodecyl phthalate 20 parts, aluminum hydroxide 15 parts;

[0021] The B component is composed of the following materials in parts by weight: 50 parts of epoxy resin, 30 parts of diisodecyl phthalate, 1.5 parts of distilled water, 0.3 parts of titanate, and 15 parts of phosphite;

[0022] The weight ratio of the component A to the component B is 4:1; the curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0023] The preparation method of the A component is as follows: the silane-terminated polyurethane resin (Wacker brand) STP-E35), silane coupling agent KH-540, antioxidant 1010, aluminum hydroxide, and diisodecyl phthalate are put into the reactor, the temperature is raised to 115°C, the vacuum degree is not less than -0.095MPa, dehydration is carried out for 1.5 hours, the temperature is lowered to below 45°C, calcium oxide and curing agent are added, stirring is carried out for 30 minutes, and then sealed and packaged.

[0024] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, phosphite and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 1 hour, and after the moisture content is tested to be within the range of 3000ppm, the material is discharged and packaged.

[0025] Example 2

[0026] A two-component silane-modified polyether-type conformal adhesive, comprising component A and component B, wherein component A is composed of the following substances in parts by weight: 50 parts of a silane-terminated polyurethane resin (SAX400 from Kaneka Chemical), 2 parts of a silane coupling agent KH-560, 2 parts of a curing agent, 0.1 parts of an antioxidant 245, 0.5 parts of xylene, 10 parts of diisononyl phthalate, and 10 parts of aluminum oxide;

[0027] The B component is composed of the following materials in parts by weight: 40 parts of epoxy resin, 20 parts of diisononyl phthalate, 1 part of distilled water, 0.1 parts of titanate, and 10 parts of polyphosphate;

[0028] The weight ratio of the component A to the component B is 3:1; the curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0029] The preparation method of the A component is as follows: end-silyl polyurethane resin (SAX400 of Zhongyuan Chemical), silane coupling agent KH-560, antioxidant 245, alumina, and diisononyl phthalate are put into a reactor according to weight, the temperature is raised to 110°C, the vacuum degree is not less than -0.095MPa, dehydration is carried out for 1 hour, the temperature is lowered to below 45°C, xylene and curing agent are added, stirring is carried out for 20 minutes, and then sealed and packaged.

[0030] The preparation method of the B component is as follows: epoxy resin, diisononyl phthalate, distilled water, polyphosphate ester and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 0.5 hours, and after the moisture content is tested to be within the range of 1000ppm, the material is discharged and packaged.

[0031] Example 3

[0032] A two-component silane-modified polyether-type conformal adhesive, comprising component A and component B, wherein component A is composed of the following substances in parts by weight: 70 parts of Zhejiang Huangma Technology's brand 12 silane-terminated polyurethane resin, 5 parts of silane coupling agent A-1120, 8 parts of curing agent, 0.5 parts of antioxidant BHT, 11 parts of water scavenger A-17, 30 parts of diisodecyl phthalate, and 20 parts of aluminum hydroxide;

[0033] The B component is composed of the following materials in parts by weight: 60 parts of epoxy resin, 40 parts of diisodecyl phthalate, 2 parts of distilled water, 0.5 parts of titanate, and 20 parts of phosphite;

[0034] The weight ratio of the component A to the component B is 5:1; the curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0035] The preparation method of the A component is as follows: Zhejiang Huangma Technology's brand 12 end-silyl polyurethane resin, silane coupling agent A-1120, antioxidant BHT, aluminum hydroxide, and diisodecyl phthalate are put into a reactor according to weight parts, the temperature is raised to 120° C., the vacuum degree is not less than -0.095 MPa, dehydration is carried out for 2 hours, the temperature is lowered to below 45° C., a dehydrating agent and a curing agent are added, the mixture is stirred for 40 minutes, and then sealed and packaged.

[0036] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, phosphite, and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 2 hours, and after the moisture content is tested to be within the range of 5000ppm, the material is discharged and packaged.

[0037] Comparative Example 1

[0038] A two-component silane-modified polyether type three-proof adhesive, comprising component A and component B, wherein component A is composed of the following materials in parts by weight: 60 parts of terminal silane-based polyurethane resin (Wacker brand STP-E35), silane coupling agent KH-540 4 parts, isophorone diamine 6 parts, antioxidant 1010 0.3 parts, calcium oxide 0.8 parts, diisodecyl phthalate 20 parts, aluminum hydroxide 15 parts;

[0039] The B component is composed of the following materials in parts by weight: 50 parts of epoxy resin, 30 parts of diisodecyl phthalate, 1.5 parts of distilled water, 0.3 parts of titanate, and 15 parts of phosphite;

[0040] The weight ratio of component A to component B is 4:1.

[0041] The preparation method of the A component is as follows: the silane-terminated polyurethane resin (Wacker brand) STP-E35), silane coupling agent KH-540, antioxidant 1010, aluminum hydroxide, and diisodecyl phthalate are put into the reaction kettle, the temperature is raised to 115°C, the vacuum degree is not less than -0.095MPa, dehydration is carried out for 1.5 hours, the temperature is lowered to below 45°C, calcium oxide and isophoronediamine are added, stirring is carried out for 30 minutes, and then sealed and packaged.

[0042] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, phosphite and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 1 hour, and after the moisture content is tested to be within the range of 3000ppm, the material is discharged and packaged.

[0043] Comparative Example 2

[0044] A two-component silane-modified polyether type three-proof adhesive, comprising component A and component B, wherein component A is composed of the following materials in parts by weight: 60 parts of terminal silane-based polyurethane resin (Wacker brand STP-E35), silane coupling agent KH-540 4 parts, 2,4,6 tris (dimethylaminomethyl) phenol 6 parts, antioxidant 1010 0.3 parts, calcium oxide 0.8 parts, diisodecyl phthalate 20 parts, aluminum hydroxide 15 parts;

[0045] The B component is composed of the following materials in parts by weight: 50 parts of epoxy resin, 30 parts of diisodecyl phthalate, 1.5 parts of distilled water, 0.3 parts of titanate, and 15 parts of phosphite;

[0046] The weight ratio of component A to component B is 4:1.

[0047] The preparation method of the A component is as follows: silane-terminated polyurethane resin (Wacker brand) STP-E35), silane coupling agent KH-540, antioxidant 1010, aluminum hydroxide, and diisodecyl phthalate are put into the reactor, the temperature is raised to 115°C, the vacuum degree is not less than -0.095 MPa, dehydration is carried out for 1.5 hours, the temperature is lowered to below 45°C, calcium oxide and 2,4,6-tris(dimethylaminomethyl)phenol are added, stirring is carried out for 30 minutes, and the reaction is sealed and packaged.

[0048] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, phosphite and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 1 hour, and after the moisture content is tested to be within the range of 3000ppm, the material is discharged and packaged.

[0049] Comparative Example 3

[0050] A two-component silane-modified polyether type three-proof adhesive, comprising component A and component B, wherein component A is composed of the following materials in parts by weight: 60 parts of terminal silane-based polyurethane resin (Wacker brand STP-E35), silane coupling agent KH-540 4 parts, curing agent 6 parts, antioxidant 10100.3 parts, calcium oxide 0.8 parts, diisodecyl phthalate 20 parts, aluminum hydroxide 30 parts;

[0051] The B component is composed of the following materials in parts by weight: 50 parts of epoxy resin, 30 parts of diisodecyl phthalate, 1.5 parts of distilled water, and 0.3 parts of titanate;

[0052] The weight ratio of the component A to the component B is 4:1; the curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0053] The preparation method of the A component is as follows: silane-terminated polyurethane resin (Wacker brand) STP-E35), silane coupling agent KH-540, antioxidant 1010, aluminum hydroxide, and diisodecyl phthalate are put into the reactor, the temperature is raised to 115°C, the vacuum degree is not less than -0.095MPa, dehydration is carried out for 1.5 hours, the temperature is lowered to below 45°C, calcium oxide and curing agent are added, stirring is carried out for 30 minutes, and then sealed and packaged.

[0054] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 1 hour, and after the moisture content is tested to be within the range of 3000ppm, the material is discharged and packaged.

[0055] Comparative Example 4

[0056] A two-component silane-modified polyether type three-proof adhesive, comprising component A and component B, wherein component A is composed of the following materials in parts by weight: 60 parts of terminal silane-based polyurethane resin (Wacker brand STP-E35), silane coupling agent KH-540 4 parts, curing agent 6 parts, antioxidant 10100.3 parts, calcium oxide 0.8 parts, diisodecyl phthalate 20 parts;

[0057] The B component is composed of the following materials in parts by weight: 50 parts of epoxy resin, 30 parts of diisodecyl phthalate, 1.5 parts of distilled water, 0.3 parts of titanate, and 30 parts of phosphite;

[0058] The weight ratio of the component A to the component B is 4:1; the curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:1.

[0059] The preparation method of the A component is as follows: silane-terminated polyurethane resin (Wacker brand) STP-E35), silane coupling agent KH-540, antioxidant 1010, and diisodecyl phthalate are put into the reactor, the temperature is raised to 115°C, the vacuum degree is not less than -0.095MPa, dehydration is carried out for 1.5 hours, the temperature is lowered to below 45°C, calcium oxide and curing agent are added, and after stirring for 30 minutes, the reaction mixture is sealed and packaged.

[0060] The preparation method of the B component is as follows: epoxy resin, diisodecyl phthalate, distilled water, phosphite and titanate are sequentially added into a reactor according to parts by weight, stirred thoroughly for 1 hour, and after the moisture content is tested to be within the range of 3000ppm, the material is discharged and packaged.

[0061] Experimental example:

[0062] The properties of the two-component silane-modified polyether-type conformal adhesive prepared in Example 1 and Comparative Examples 1-4 were measured. The open-drying time was tested according to GB / T13477; the tensile strength and elongation at break were tested according to GB / T528; the viscosity test was carried out according to the rotation test method in GBT22235-2008; the hardness was tested according to HG T 2368-2011; the volume resistivity was tested according to GB / T1410-2006; the water resistance was tested according to GB / T1733-1993; and the salt spray resistance was tested according to GB / T2423.17-2008.

[0063] Table 1

[0064]

[0065] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A two-component silane-modified polyether type three-proof adhesive, characterized in that: The invention comprises component A and component B, wherein component A is composed of the following substances in parts by weight: 50-70 parts of a silane-terminated polyurethane resin, 1-5 parts of a silane coupling agent, 1-8 parts of a curing agent, 0.1-0.5 parts of an antioxidant, 0.5-1 parts of a water scavenger, 10-30 parts of a plasticizer, and 10-20 parts of aluminum hydroxide; The B component is composed of the following materials in parts by weight: 40-60 parts of epoxy resin, 20-40 parts of plasticizer, 1-2 parts of distilled water, 0.1-0.5 parts of catalyst, and 10-20 parts of phosphite; The weight ratio of component A to component B is (2.5-5):1; The curing agent is a mixture of isophorone diamine and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:

1.

2. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The terminal silane-based polyurethane resins are Wacker's GENIOSIL® STP-E35 and GENIOSIL® STP-E15 terminal silane-based polyurethane resins; Zhongyuan Chemical's SAX400 and SAX750 terminal silane-based polyurethane resins; Zhejiang Huangma Technology's brand 12 terminal silane-based polyurethane resin; and Ruiyang Antai's brand 30 terminal silane-based polyurethane resin.

3. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The silane coupling agent is one or more of KH-540, KH-550, KH-560, KH-570, A-1120, and A-1146.

4. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The antioxidant is one or more of antioxidants 1010, 245, and BHT; the dehydrating agent is one or more of calcium oxide, xylene, and dehydrating agent A-171; and the plasticizer is diisodecyl phthalate and / or diisononyl phthalate.

5. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The catalyst is titanate.

6. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The preparation method of the A component is as follows: end-silyl polyurethane resin, silane coupling agent, antioxidant, aluminum hydroxide, and plasticizer are added into a reaction kettle according to parts by weight, the temperature is raised to 110-120° C., the vacuum degree is not less than -0.095 MPa, dehydration is performed for 1-2 hours, the temperature is lowered to below 45° C., a dehydrating agent and a curing agent are added, the mixture is stirred for 20-40 minutes, and then sealed and packaged.

7. The two-component silane-modified polyether-type conformal adhesive according to claim 1, characterized in that: The preparation method of the B component is as follows: epoxy resin, plasticizer, distilled water, phosphite, and catalyst are sequentially added into a reactor according to parts by weight, stirred thoroughly for 0.5-2 hours, and after the moisture content is tested to be within the range of 1000-5000 ppm, the material is discharged and packaged.

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