High-wear-resistance photocuring aromatic ether-based epoxy acrylate/nanosilicon dioxide composite material and preparation method thereof

Abstract

The invention discloses an aromatic ether-based epoxy acrylate / nanosilicon dioxide composite material and a preparation method and applications thereof. The preparation method comprises the following steps: synthesizing a bisphenol compound of an aromatic ether ketone chain segment based on substitution reaction, performing reduction of carbonyl, phenolic hydroxyl epoxy acylation, and bridging of isocyanate group of alcoholic hydroxyl group, to prepare a four-degree-functionality epoxy acrylate compound, then mixing sulfdryl-modified nanosilicon dioxide particles, and performing ultraviolet photocuring to prepare an aromatic ether-based epoxy acrylate / nanosilicon dioxide composite material. The method is simple to operate, convenient and easy. Compared with a pure acrylate material, the composite material has the advantages of high wear resistance, high hardness, excellent thermal / chemical stability and the like after being subjected to ultraviolet photocuring, thus having wide industrial application prospects.

Description

technical field

[0001] The invention belongs to the field of inorganic / organic polymer composite materials, and in particular relates to a high wear-resistant light-cured aryl ether-based epoxy acrylate / nano silicon dioxide composite material and a preparation method thereof. Background technique

[0002] With the development of society and the increase in demand for high-end markets such as electronic appliances, the existing epoxy acrylic light-curing resins have disadvantages such as low hardness, easy scratching of the surface, poor wear resistance, easy water absorption and poor solvent resistance. It has become increasingly prominent. Therefore, it is urgent to develop a series of high-performance photocurable resins such as high temperature resistance and wear resistance to meet the needs of the high-end market. Due to the special properties of nanomaterials, adding inorganic nanoparticles to the coating can greatly improve the wear resistance of the coating, and can ...

Examples

Embodiment 1

[0049] Embodiment 1 hydroquinone type photocurable epoxy acrylate / nano silicon dioxide composite material

[0050] (1) Preparation of aryl ether ketone bisphenols based on hydroquinone: equipped with condenser, water separator, mechanical stirring and N 2 160mmol of hydroquinone, 80mmol of 4,4-difluorobenzophenone, 192mmol of potassium carbonate, 160mL of DMSO and 20mL of toluene were added to the dry three-necked flask of the catheter. in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then evaporated the water-carrying agent, and reacted at 175°C for 10h. The product was settled in 1000 mL of distilled water, filtered, and then vacuum-dried at 60° C. for 48 hours to obtain bisphenol containing aryl ether ketone segments in the form of yellow-white powder with a yield of 96%.

[0051] (2) Preparation of aryl ether alcohol-containing bisphenols based on hydroquinone: in a dry three-necked flask, add...

Embodiment 2

[0057] Embodiment 2 Bisphenol A type photocurable epoxy acrylate / nano silicon dioxide composite material

[0058] (1) Preparation of aryl ether ketone bisphenols based on bisphenol A: when equipped with reflux condenser, water separator, mechanical stirring and N 2 Into the dry three-necked flask of the introduction tube, add 160mmol of bisphenol A, 80mmol of 4,4-difluorobenzophenone, 200mmol of potassium carbonate, 160mL of DMSO and 120mL of toluene. in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then evaporated the water-carrying agent, and reacted at 175°C for 10h. The product was settled in 1000 mL of distilled water, filtered, and then vacuum-dried at 60° C. for 48 hours to obtain bisphenol containing aryl ether ketone segment in the form of white powder with a yield of 94%.

[0059] (2) Preparation of bisphenol containing aryl ether alcohol based on bisphenol A: 120mmol NaBH 4 Add to 50mL...

Embodiment 3

[0065] Embodiment 3 is based on biphenol and bisphenol S type photocurable epoxy acrylate / nanometer silicon dioxide composite material

[0066] (1) Preparation of aryl ether ketone bisphenols based on biphenol and bisphenol S: in a dry three-necked flask, add biphenol 80mmol and bisphenol S 80mmol, 4,4-difluorobenzophenone 80mmol, potassium carbonate 200mmol, 160mLDMSO and 120mL toluene were mixed homogeneously, in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then raised the temperature to 175°C to distill the water-carrying agent toluene, and reacted at 175°C for 10h. The product was extracted three times with a small amount of chloroform and an appropriate amount of distilled water, and the organic phase was taken, and the solvent was removed by rotary evaporation at 60°C, and then vacuum-dried at 60°C for 48 hours to obtain a white solid powder containing a bisphenol monomer containing an aryl e...

technical field

[0001] The invention belongs to the field of inorganic / organic polymer composite materials, and in particular relates to a high wear-resistant light-cured aryl ether-based epoxy acrylate / nano silicon dioxide composite material and a preparation method thereof. Background technique

[0002] With the development of society and the increase in demand for high-end markets such as electronic appliances, the existing epoxy acrylic light-curing resins have disadvantages such as low hardness, easy scratching of the surface, poor wear resistance, easy water absorption and poor solvent resistance. It has become increasingly prominent. Therefore, it is urgent to develop a series of high-performance photocurable resins such as high temperature resistance and wear resistance to meet the needs of the high-end market. Due to the special properties of nanomaterials, adding inorganic nanoparticles to the coating can greatly improve the wear resistance of the coating, and can ...

Examples

Embodiment 1

[0049] Embodiment 1 hydroquinone type photocurable epoxy acrylate / nano silicon dioxide composite material

[0050] (1) Preparation of aryl ether ketone bisphenols based on hydroquinone: equipped with condenser, water separator, mechanical stirring and N 2 160mmol of hydroquinone, 80mmol of 4,4-difluorobenzophenone, 192mmol of potassium carbonate, 160mL of DMSO and 20mL of toluene were added to the dry three-necked flask of the catheter. in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then evaporated the water-carrying agent, and reacted at 175°C for 10h. The product was settled in 1000 mL of distilled water, filtered, and then vacuum-dried at 60° C. for 48 hours to obtain bisphenol containing aryl ether ketone segments in the form of yellow-white powder with a yield of 96%.

[0051] (2) Preparation of aryl ether alcohol-containing bisphenols based on hydroquinone: in a dry three-necked flask, add...

Embodiment 2

[0057] Embodiment 2 Bisphenol A type photocurable epoxy acrylate / nano silicon dioxide composite material

[0058] (1) Preparation of aryl ether ketone bisphenols based on bisphenol A: when equipped with reflux condenser, water separator, mechanical stirring and N 2 Into the dry three-necked flask of the introduction tube, add 160mmol of bisphenol A, 80mmol of 4,4-difluorobenzophenone, 200mmol of potassium carbonate, 160mL of DMSO and 120mL of toluene. in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then evaporated the water-carrying agent, and reacted at 175°C for 10h. The product was settled in 1000 mL of distilled water, filtered, and then vacuum-dried at 60° C. for 48 hours to obtain bisphenol containing aryl ether ketone segment in the form of white powder with a yield of 94%.

[0059] (2) Preparation of bisphenol containing aryl ether alcohol based on bisphenol A: 120mmol NaBH 4 Add to 50mL...

Embodiment 3

[0065] Embodiment 3 is based on biphenol and bisphenol S type photocurable epoxy acrylate / nanometer silicon dioxide composite material

[0066] (1) Preparation of aryl ether ketone bisphenols based on biphenol and bisphenol S: in a dry three-necked flask, add biphenol 80mmol and bisphenol S 80mmol, 4,4-difluorobenzophenone 80mmol, potassium carbonate 200mmol, 160mLDMSO and 120mL toluene were mixed homogeneously, in N 2 Heated under the protection of the reactant until the reactants were dissolved, refluxed and dehydrated at 150°C for 2h, then raised the temperature to 175°C to distill the water-carrying agent toluene, and reacted at 175°C for 10h. The product was extracted three times with a small amount of chloroform and an appropriate amount of distilled water, and the organic phase was taken, and the solvent was removed by rotary evaporation at 60°C, and then vacuum-dried at 60°C for 48 hours to obtain a white solid powder containing a bisphenol monomer containing an aryl e...

Images