Dual-curable polysiloxane as well as preparation method and application thereof

Abstract

The invention discloses double-curable polysiloxane as well as a preparation method and application thereof. Acrylate groups contained in the molecular structure of polysiloxane can be quickly cross-linked and cured under the condition of ultraviolet irradiation, and moisture curing groups are contained in the end group structure, so that the polymer has moisture curing and UV light curing capabilities at the same time. According to a synthetic route provided by the invention, generation of acrylate can be avoided, silicon hydroxyl residue is lower than 1%, energy required by photocuring of the polymer is reduced, and the damp-heat aging resistance of a cured product is improved.

Description

technical field

[0001] The invention relates to a dual-curable polysiloxane, a preparation method and application thereof, and belongs to the field of silicon materials. Background technique

[0002] The unique molecular structure of silicone makes it have the properties of both inorganic materials and organic materials. It has excellent properties such as oxidation resistance, weather resistance, flame retardancy, water repellency, corrosion resistance, and physiological inertness. It is widely used in electronic circuits Protection of panels and main components.

[0003] UV curing technology has the characteristics of fast curing, energy saving, room temperature curing, less pollution, and superior performance. It is a new generation of green chemical technology. The photosensitive group is introduced into the polysiloxane molecular chain to make it a photocurable polysiloxane to improve its curing efficiency, which not only saves energy but also reduces environmental pol...

Examples

Embodiment 1

[0046] Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 70cP, start stirring at 300r / min, vacuumize at 80°C to remove water for 60min, cool down to 50°C, add 23g of dimethoxydi Chloropropylsilane, after stirring for 15min, add 0.7g of acetic acid, react for 3h, add 46g of chloropropyltrimethoxysilane, react for 2h, extract the low boiling point at 100°C and 5mbar, add p-hydroxyanisole 0.015 g, 20g of sodium acrylate, stir well, add 2.5g of tetramethylammonium hydroxide and raise the temperature to 80°C for 3 hours, then raise the temperature to 150°C, extract the low boiling point under the condition of 5mbar, and filter under positive pressure to obtain the product I. After testing its silanol The residue was 0.7%, methyl acrylate was not detected.

Embodiment 2

[0048]Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 200cP, start stirring at 300r / min, vacuumize at 100°C to remove water for 60min, cool down to 60°C, add 18g of dimethoxydi Chloropropylsilane, after stirring for 15min, add 0.5g of phosphoric acid, react for 3h, add 38g of chloropropyltrimethoxysilane, react for 2h, extract the low boiling point at 100℃, 5mbar, and add N,N-diethyl Hydroxylamine 0.01g, sodium acrylate 16g, stir evenly, add 2.5g tetramethylammonium hydroxide and heat up to 80°C for 3 hours, then heat up to 145°C, extract low boiling point under 5mbar, and filter under positive pressure to obtain product II. After testing Its silanol residue was 0.8%, and methyl acrylate was not detected.

Embodiment 3

[0050] Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 100cP, start stirring at 300r / min, vacuumize at 90°C to remove water for 60min, cool down to 70°C, add 20.5g of dimethoxy Dichloropropylsilane, after stirring for 15min, add 0.6g phosphoric acid, react for 4h, add 42g chloropropyltrimethoxysilane, react for 3h, extract the low boiling point at 110°C and 6mbar, add p-hydroxyanisole to the obtained product 0.015g, 18g of sodium acrylate, stir well, add 2.6g of tetramethylammonium hydroxide and raise the temperature to 80°C for 4 hours, then raise the temperature to 150°C, extract the low boiling point under the condition of 5mbar, and filter under positive pressure to obtain the product III. After testing its silicon The residual hydroxyl group was 0.6%, and methyl acrylate was not detected.

technical field

[0001] The invention relates to a dual-curable polysiloxane, a preparation method and application thereof, and belongs to the field of silicon materials. Background technique

[0002] The unique molecular structure of silicone makes it have the properties of both inorganic materials and organic materials. It has excellent properties such as oxidation resistance, weather resistance, flame retardancy, water repellency, corrosion resistance, and physiological inertness. It is widely used in electronic circuits Protection of panels and main components.

[0003] UV curing technology has the characteristics of fast curing, energy saving, room temperature curing, less pollution, and superior performance. It is a new generation of green chemical technology. The photosensitive group is introduced into the polysiloxane molecular chain to make it a photocurable polysiloxane to improve its curing efficiency, which not only saves energy but also reduces environmental pol...

Examples

Embodiment 1

[0046] Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 70cP, start stirring at 300r / min, vacuumize at 80°C to remove water for 60min, cool down to 50°C, add 23g of dimethoxydi Chloropropylsilane, after stirring for 15min, add 0.7g of acetic acid, react for 3h, add 46g of chloropropyltrimethoxysilane, react for 2h, extract the low boiling point at 100°C and 5mbar, add p-hydroxyanisole 0.015 g, 20g of sodium acrylate, stir well, add 2.5g of tetramethylammonium hydroxide and raise the temperature to 80°C for 3 hours, then raise the temperature to 150°C, extract the low boiling point under the condition of 5mbar, and filter under positive pressure to obtain the product I. After testing its silanol The residue was 0.7%, methyl acrylate was not detected.

Embodiment 2

[0048]Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 200cP, start stirring at 300r / min, vacuumize at 100°C to remove water for 60min, cool down to 60°C, add 18g of dimethoxydi Chloropropylsilane, after stirring for 15min, add 0.5g of phosphoric acid, react for 3h, add 38g of chloropropyltrimethoxysilane, react for 2h, extract the low boiling point at 100℃, 5mbar, and add N,N-diethyl Hydroxylamine 0.01g, sodium acrylate 16g, stir evenly, add 2.5g tetramethylammonium hydroxide and heat up to 80°C for 3 hours, then heat up to 145°C, extract low boiling point under 5mbar, and filter under positive pressure to obtain product II. After testing Its silanol residue was 0.8%, and methyl acrylate was not detected.

Embodiment 3

[0050] Take a 1000ml four-neck flask and dry it fully, add 500g of hydroxyl-terminated polysiloxane with a viscosity of 100cP, start stirring at 300r / min, vacuumize at 90°C to remove water for 60min, cool down to 70°C, add 20.5g of dimethoxy Dichloropropylsilane, after stirring for 15min, add 0.6g phosphoric acid, react for 4h, add 42g chloropropyltrimethoxysilane, react for 3h, extract the low boiling point at 110°C and 6mbar, add p-hydroxyanisole to the obtained product 0.015g, 18g of sodium acrylate, stir well, add 2.6g of tetramethylammonium hydroxide and raise the temperature to 80°C for 4 hours, then raise the temperature to 150°C, extract the low boiling point under the condition of 5mbar, and filter under positive pressure to obtain the product III. After testing its silicon The residual hydroxyl group was 0.6%, and methyl acrylate was not detected.

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