Preparation method of high-transparency flexible flame-retardant film

Abstract

The invention provides a preparation method of a high-transparency flexible flame-retardant film, and belongs to the field of flexible flame-retardant films. The preparation method comprises the following steps: preparing an intermediate A; preparing an intermediate B; preparing an intermediate C; adding polyvinyl alcohol into distilled water; raising the temperature to 90 to 95 DEG C and stirringfor 5 to 10min to obtain a polyvinyl alcohol solution with a certain mass concentration, cooling to 50 to 60 DEG C, adding the intermediate A and the intermediate C; keeping the temperature and stirring for 30 to 40min, then, adding nano cellulose and natural clay, continuously stirring for 1-3h, after vacuum defoaming, carrying out film coating on a flat glass plate, transferring the glass plateinto a drying oven with the temperature of 40 to 50 DEG C and drying for 2 to 5h; and heating to 80 to 85 DEG C for 5 to 10h of curing to obtain the high-transparency flexible flame-retardant film which is high in elongation at break, small in Young modulus, excellent in flexibility and good in transparency, the light transmittance reaches 96.5%, and the high-transparency flexible flame-retardantfilm has excellent flame-retardant performance.

Description

technical field

[0001] The invention relates to the field of flexible flame-retardant films, in particular to a preparation method of highly transparent flexible flame-retardant films. Background technique

[0002] The industrial trend of the rise of flexible electronics has become increasingly clear, and products such as flexible displays, flexible lighting, flexible solar cells, and flexible sensors have gradually moved from the laboratory to the market. Under this industry trend, soft transparent conductive films with flexibility, high light penetration, and high conductivity are the basis of many flexible optoelectronic products. Therefore, flexible transparent conductive films will become a strategic material for flexible optoelectronic products. With the development of flexibility, thinning and light weight of electronic devices, flexible transparent films have broad application prospects in flexible batteries, displays, touch screens and other wearable electronic dev...

Examples

Embodiment 1

[0028] A preparation method of a highly transparent and flexible flame-retardant film:

[0029] Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.1, and heat up to 80°C for reaction After 5 hours, raise the temperature to 120°C, continue the reaction for 3 hours, add the terminator benzoic acid, then raise the temperature to 140°C for 2 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, heat up to 40°C and stir After making it dissolve, slowly add a certain amount of distilled water. The weight ratio of cyclic phosphoric anhydride to distilled water is 7:1. Mix 1:0.8:0.13, raise the temperature to reflux for 10 hours, filter, and mix the obtained solid with absolute ethanol in a weight ratio of 1:10 at room temperature for 2 hours, filter, and concentrate and dry the filtrate under reduced pressure to obtain intermediate B...

Embodiment 2

[0031] A preparation method of a highly transparent and flexible flame-retardant film:

[0032]Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.2, and heat up to 90°C for reaction After 5 hours, raise the temperature to 120°C, continue the reaction for 2 hours, add the terminator hydroquinone, then raise the temperature to 140°C for 3 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, and heat up to 50 Stir at ℃ to make it dissolve, then slowly add a certain amount of distilled water dropwise, the weight ratio of cyclic phosphoric anhydride to distilled water is 7:1, keep warm for 5 hours after dropping, filter, and dry the product in vacuum with hydroxyethyl acrylate and cationic resin Mix at a weight ratio of 1:0.8:0.13, heat up to reflux for 10 hours, filter, and filter the obtained solid and absolute ethanol at a weig...

Embodiment 3

[0034] A preparation method of a highly transparent and flexible flame-retardant film:

[0035] Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.2, and heat up to 90°C for reaction After 3-5 hours, raise the temperature to 120°C, continue the reaction for 2 hours, add the terminator hydroquinone, then raise the temperature to 140°C for 3 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, and heat up Stir at 50°C to make it dissolve, then slowly add a certain amount of distilled water dropwise, the weight ratio of cyclic phosphoric anhydride to distilled water is 7:1, keep warm for 3 hours after dropping, filter, and dry the product in vacuum with hydroxyethyl acrylate, cationic The resin is mixed at a weight ratio of 1:0.8:0.13, heated to reflux for 10 hours, filtered, and the solid obtained by filtering is mixed with abs...

technical field

[0001] The invention relates to the field of flexible flame-retardant films, in particular to a preparation method of highly transparent flexible flame-retardant films. Background technique

[0002] The industrial trend of the rise of flexible electronics has become increasingly clear, and products such as flexible displays, flexible lighting, flexible solar cells, and flexible sensors have gradually moved from the laboratory to the market. Under this industry trend, soft transparent conductive films with flexibility, high light penetration, and high conductivity are the basis of many flexible optoelectronic products. Therefore, flexible transparent conductive films will become a strategic material for flexible optoelectronic products. With the development of flexibility, thinning and light weight of electronic devices, flexible transparent films have broad application prospects in flexible batteries, displays, touch screens and other wearable electronic dev...

Examples

Embodiment 1

[0028] A preparation method of a highly transparent and flexible flame-retardant film:

[0029] Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.1, and heat up to 80°C for reaction After 5 hours, raise the temperature to 120°C, continue the reaction for 3 hours, add the terminator benzoic acid, then raise the temperature to 140°C for 2 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, heat up to 40°C and stir After making it dissolve, slowly add a certain amount of distilled water. The weight ratio of cyclic phosphoric anhydride to distilled water is 7:1. Mix 1:0.8:0.13, raise the temperature to reflux for 10 hours, filter, and mix the obtained solid with absolute ethanol in a weight ratio of 1:10 at room temperature for 2 hours, filter, and concentrate and dry the filtrate under reduced pressure to obtain intermediate B...

Embodiment 2

[0031] A preparation method of a highly transparent and flexible flame-retardant film:

[0032]Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.2, and heat up to 90°C for reaction After 5 hours, raise the temperature to 120°C, continue the reaction for 2 hours, add the terminator hydroquinone, then raise the temperature to 140°C for 3 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, and heat up to 50 Stir at ℃ to make it dissolve, then slowly add a certain amount of distilled water dropwise, the weight ratio of cyclic phosphoric anhydride to distilled water is 7:1, keep warm for 5 hours after dropping, filter, and dry the product in vacuum with hydroxyethyl acrylate and cationic resin Mix at a weight ratio of 1:0.8:0.13, heat up to reflux for 10 hours, filter, and filter the obtained solid and absolute ethanol at a weig...

Embodiment 3

[0034] A preparation method of a highly transparent and flexible flame-retardant film:

[0035] Add hydrazine sulfate, terephthalic acid, and 5-bromoisophthalic acid to oleum, wherein the weight ratio of terephthalic acid and 5-bromoisophthalic acid is 1:0.2, and heat up to 90°C for reaction After 3-5 hours, raise the temperature to 120°C, continue the reaction for 2 hours, add the terminator hydroquinone, then raise the temperature to 140°C for 3 hours, obtain intermediate A after vacuum defoaming, add cyclic phosphoric anhydride to acetone, and heat up Stir at 50°C to make it dissolve, then slowly add a certain amount of distilled water dropwise, the weight ratio of cyclic phosphoric anhydride to distilled water is 7:1, keep warm for 3 hours after dropping, filter, and dry the product in vacuum with hydroxyethyl acrylate, cationic The resin is mixed at a weight ratio of 1:0.8:0.13, heated to reflux for 10 hours, filtered, and the solid obtained by filtering is mixed with abs...

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