CN112080213A - Preparation method of flame-retardant light-storing film - Google Patents
Preparation method of flame-retardant light-storing film Download PDFInfo
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- CN112080213A CN112080213A CN202010896017.5A CN202010896017A CN112080213A CN 112080213 A CN112080213 A CN 112080213A CN 202010896017 A CN202010896017 A CN 202010896017A CN 112080213 A CN112080213 A CN 112080213A
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
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Abstract
The utility model provides a preparation method of fire-retardant type light-storing film, light-storing film include transparent fire-retardant protective layer, light-storing layer, light shield layer, gum layer and release paper layer that from the top down set gradually, and transparent fire-retardant protective layer includes following raw materials: the transparent flame-retardant protective layer is characterized by comprising PET, triphenyl phosphate, epoxidized soybean oil, triethyl phosphoryl acetate, ammonium polyphosphate, molybdenum trioxide, zirconium hydroxide, zinc oxide and lauryl methacrylate, wherein triphenyl phosphate, the ammonium polyphosphate, the molybdenum trioxide, the zirconium oxide and the zinc oxide are added to cooperate with one another, so that the smoke generation amount of the finally formed light-storage film is reduced by 50-80%, the oxygen index is improved by 40-55%, the effect of self-extinguishing after leaving fire is achieved, the flame retardance is detected according to UL94, and the flame-retardant grade of the light-storage film can reach V-0 level.
Description
Technical Field
The invention belongs to the field of light storage film preparation, and particularly relates to a preparation method of a flame-retardant light storage film.
Background
The light storage film is a film with a certain thickness formed by combining a high polymer material and light storage powder and adopting an extrusion or coating process, is widely applied to the fields of subways, shopping malls, high-rise safety channels, house numbers and the like, and plays a role in showing and guiding in the dark; the current popular light storage film has the main structure that: the light-emitting diode comprises a surface layer, a light-storing layer, a light-shielding layer, a back glue layer and a release paper layer.
The national requirement for indoor fire prevention of buildings is increasingly increased, and some places put forward the requirement for fire prevention and flame retardance for indoor safety guide marks of buildings, so that the light storage film for manufacturing the marks is required to have flame retardance; the flame-retardant light-storing film requires flame retardance and cannot reduce the reflective performance and other physical properties.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a flame-retardant light-storing film.
The invention adopts the following technical scheme:
the utility model provides a preparation method of fire-retardant type light-storing film, light-storing film include transparent fire-retardant protective layer, light-storing layer, light shield layer, gum layer and release paper layer that from the top down set gradually, and transparent fire-retardant protective layer includes the raw materials of following parts by weight: PET90-110 parts, triphenyl phosphate 25-35 parts, epoxidized soybean oil 5-10 parts, triethyl phosphonoacetate 2-3 parts, ammonium polyphosphate 5-10 parts, molybdenum trioxide 6-10 parts, zirconium hydroxide 12-18 parts, zinc oxide 8-12 parts, and lauryl methacrylate 1-3 parts;
the preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 80-100s at 70-80 ℃ to form a light-storing layer;
step two, coating shading slurry on the bottom surface of the light storage layer, and drying to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 50-60 ℃ for 90-100s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying and compounding with the shading layer to form the flame-retardant light storage film.
Further, the light-storing ink is prepared from the following raw materials in parts by weight: 18-25 parts of white ink, 12-18 parts of acrylic resin, 5-8 parts of methyl isobutyl ketone, 8-12 parts of diethylene glycol ethyl ether, 2-4 parts of trimethyl hexamethylene diamine, 3-5 parts of a flame retardant and 30-35 parts of a light-storing liquid.
Further, the flame retardant consists of the following raw materials in parts by weight: 20-25 parts of zinc borate, 15-22 parts of zinc oxide, 10-18 parts of zinc dihydrogen phosphate, 10-20 parts of aluminum hydroxide, 5-10 parts of magnesium chloride, 8-12 parts of kieselguhr and 3-5 parts of ammonium polyphosphate.
Further, the light storage liquid is formed by mixing zinc sulfide, varnish and ethanol according to the weight ratio of 10:10: 3.
Further, the back glue layer comprises the following raw materials in parts by weight: 60-70 parts of water-based acrylic resin, 20-25 parts of clam powder, 3-5 parts of polypropylene glycol, 0.3-0.5 part of flatting agent, 0.2-0.5 part of defoaming agent and 20-30 parts of deionized water.
Further, the method for preparing the light storage ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at the normal temperature and the rotating speed of 1000-2000r/min for 60-70 min; and then, continuously adding the light storage liquid and the flame retardant, and stirring for 50-60min at the rotating speed of 1000-2000r/min to obtain the light storage ink.
Further, in the first step, the coating thickness of the light-storing ink is 1-2 filaments.
Further, in the fourth step, the composite environment of the back adhesive layer and the light shielding layer is as follows: the temperature is 90-110 ℃ and the time is 20-30 s.
As can be seen from the above description of the present invention, compared with the prior art, the beneficial effects of the present invention are: the transparent flame-retardant protective layer is added with triphenyl phosphate to be cooperatively matched with ammonium polyphosphate, molybdenum trioxide, zirconium oxide and zinc oxide, so that the smoke generation amount of the finally formed light-storing film is reduced by 50-80%, the oxygen index is improved by 40-55%, the effect of self-extinguishing after leaving fire is achieved, the flame-retardant property is detected according to UL94, and the flame-retardant grade of the light-storing film can reach V-0 level; the epoxy soybean oil is cooperatively matched with other components, so that the transparent flame-retardant protective layer has excellent heat resistance, and the service life of the light-storing film is ensured; meanwhile, triphenyl phosphate is matched with the phosphoryl triethyl acetate, so that the PET can be prevented from being degraded, the use of the light storage film is prolonged, and the light storage film also has a certain antioxidation effect, so that the protective layer is prevented from being degraded and discolored;
the flame retardant in the light storage ink can improve the oxygen index of a light storage layer by 10-20% by matching zinc borate, zinc oxide, zinc dihydrogen phosphate, aluminum hydroxide, magnesium chloride, diatomite and ammonium polyphosphate so as to improve the flame retardant property of a light storage film.
Detailed Description
The invention is further described below by means of specific embodiments.
The flame-retardant light-storing film comprises a transparent flame-retardant protective layer, a light-storing layer, a light-shielding layer, a back adhesive layer and a release paper layer which are sequentially arranged from top to bottom.
The transparent flame-retardant protective layer comprises the following raw materials in parts by weight: PET90-110 parts, triphenyl phosphate 25-35 parts, epoxidized soybean oil 5-10 parts, triethyl phosphonoacetate 2-3 parts, ammonium polyphosphate 5-10 parts, molybdenum trioxide 6-10 parts, zirconium hydroxide 12-18 parts, zinc oxide 8-12 parts, and lauryl methacrylate 1-3 parts.
The flame retardant consists of the following raw materials in parts by weight: 20-25 parts of zinc borate, 15-22 parts of zinc oxide, 10-18 parts of zinc dihydrogen phosphate, 10-20 parts of aluminum hydroxide, 5-10 parts of magnesium chloride, 8-12 parts of kieselguhr and 3-5 parts of ammonium polyphosphate.
The light-storing ink consists of the following raw materials in parts by weight: 18-25 parts of white ink, 12-18 parts of acrylic resin, 5-8 parts of methyl isobutyl ketone, 8-12 parts of diethylene glycol ethyl ether, 2-4 parts of trimethyl hexamethylene diamine, 3-5 parts of a flame retardant and 30-35 parts of light-storing liquid, wherein the light-storing liquid is prepared by mixing zinc sulfide, varnish and ethanol according to a weight ratio of 10:10: 3.
The back glue layer comprises the following raw materials in parts by weight: 60-70 parts of water-based acrylic resin, 20-25 parts of clam powder, 3-5 parts of polypropylene glycol, 0.3-0.5 part of flatting agent, 0.2-0.5 part of defoaming agent and 20-30 parts of deionized water, wherein the flatting agent is a YZ-1500 organosilicon flatting agent produced by Jiaxing polygala tenuifolia chemical company Limited; the polyether type defoaming agent is XAMA-3c polyether type defoaming agent produced by German BELL chemical industry.
The preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 80-100s at 70-80 ℃ to form a light-storing layer;
coating shading slurry on the bottom surface of the light storage layer, and drying at 60-70 ℃ to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 50-60 ℃ for 90-100s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying at 60-70 ℃, and compounding with the shading layer at 90-110 ℃ for 20-30s to form the flame-retardant light-storing film.
Specifically, the preparation method of the light-storing ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at the normal temperature and the rotating speed of 1000-2000r/min for 60-70 min; and then, continuously adding the light storage liquid and the flame retardant, and stirring for 50-60min at the rotating speed of 1000-2000r/min to obtain the light storage ink.
In the first step, the coating thickness of the light-storing ink is 1-2 filaments.
Example 1
The flame-retardant light-storing film comprises a transparent flame-retardant protective layer, a light-storing layer, a light-shielding layer, a back adhesive layer and a release paper layer which are sequentially arranged from top to bottom.
The transparent flame-retardant protective layer comprises the following raw materials in parts by weight: PET90 parts, triphenyl phosphate 35 parts, epoxidized soybean oil 5 parts, triethyl phosphoryl acetate 3 parts, ammonium polyphosphate 5 parts, molybdenum trioxide 10 parts, zirconium hydroxide 12 parts, zinc oxide 12 parts, and lauryl methacrylate 3 parts.
The flame retardant consists of the following raw materials in parts by weight: 20 parts of zinc borate, 22 parts of zinc oxide, 10 parts of zinc dihydrogen phosphate, 20 parts of aluminum hydroxide, 5 parts of magnesium chloride, 12 parts of diatomite and 3 parts of ammonium polyphosphate.
The light-storing ink consists of the following raw materials in parts by weight: 18 parts of white ink, 18 parts of acrylic resin, 5 parts of methyl isobutyl ketone, 12 parts of diethylene glycol ethyl ether, 2 parts of trimethyl hexamethylene diamine, 5 parts of a flame retardant and 30 parts of a light-storing liquid, wherein the light-storing liquid is prepared by mixing zinc sulfide, varnish and ethanol according to a weight ratio of 10:10: 3.
The back glue layer comprises the following raw materials in parts by weight: 60 parts of water-based acrylic resin, 25 parts of clam meal, 3 parts of polypropylene glycol, 0.5 part of flatting agent, 0.2 part of defoaming agent and 20 parts of deionized water.
The preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 100s at 70 ℃ to form a light-storing layer;
coating shading slurry on the bottom surface of the light storage layer, and drying at 60 ℃ to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 60 ℃ for 90s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying at 70 ℃, and compounding with the shading layer at the temperature of 90 ℃ for 30s to form the flame-retardant light-storing film.
Specifically, the preparation method of the light-storing ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at normal temperature and the rotating speed of 1000r/min for 70 min; and then, continuously adding the light storage liquid and the flame retardant, and stirring for 50min at the rotating speed of 12000r/min to obtain the light storage ink.
In the first step, the coating thickness of the light-storing ink is 1 filament.
The light-emitting film obtained in example 1 was subjected to flame retardancy test according to UL94, and after two 10-second burning tests, the flame was extinguished within 10 seconds, and no burning material was dropped, and the flame retardancy rating reached V-0 rating.
Example 2
The flame-retardant light-storing film comprises a transparent flame-retardant protective layer, a light-storing layer, a light-shielding layer, a back adhesive layer and a release paper layer which are sequentially arranged from top to bottom.
The transparent flame-retardant protective layer comprises the following raw materials in parts by weight: 110 parts of PET, 25 parts of triphenyl phosphate, 10 parts of epoxidized soybean oil, 2 parts of triethyl phosphoryl acetate, 10 parts of ammonium polyphosphate, 6 parts of molybdenum trioxide, 18 parts of zirconium hydroxide, 8 parts of zinc oxide and 1 part of lauryl methacrylate.
The flame retardant consists of the following raw materials in parts by weight: 25 parts of zinc borate, 15 parts of zinc oxide, 18 parts of zinc dihydrogen phosphate, 10 parts of aluminum hydroxide, 10 parts of magnesium chloride, 8 parts of diatomite and 5 parts of ammonium polyphosphate.
The light-storing ink consists of the following raw materials in parts by weight: 25 parts of white ink, 12 parts of acrylic resin, 8 parts of methyl isobutyl ketone, 8 parts of diethylene glycol ethyl ether, 4 parts of trimethyl hexamethylene diamine, 3 parts of a flame retardant and 35 parts of a light-storing liquid, wherein the light-storing liquid is prepared by mixing zinc sulfide, varnish and ethanol according to a weight ratio of 10:10: 3.
The back glue layer comprises the following raw materials in parts by weight: 70 parts of water-based acrylic resin, 20 parts of clam powder, 5 parts of polypropylene glycol, 0.3 part of flatting agent, 0.5 part of defoaming agent and 30 parts of deionized water.
The preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 80s at 80 ℃ to form a light-storing layer;
coating shading slurry on the bottom surface of the light storage layer, and drying at 70 ℃ to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 50 ℃ for 100s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying at 60 ℃, and compounding with the shading layer at 110 ℃ for 20s to form the flame-retardant light-storing film.
Specifically, the preparation method of the light-storing ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at the normal temperature and the rotating speed of 2000r/min for 60 min; and then, continuously adding the light storage liquid and the flame retardant, and stirring for 60min at the rotating speed of 1000r/min to obtain the light storage ink.
In the first step, the coating thickness of the light-storing ink is 2 filaments.
The light-storing film prepared in example 2 was subjected to flame retardancy test according to UL94, and after two 10-second burning tests, the flame was extinguished within 10 seconds, and no burning material was dropped, and the flame retardancy grade reached V-0 grade.
Example 3
The flame-retardant light-storing film comprises a transparent flame-retardant protective layer, a light-storing layer, a light-shielding layer, a back adhesive layer and a release paper layer which are sequentially arranged from top to bottom.
The transparent flame-retardant protective layer comprises the following raw materials in parts by weight: 100 parts of PET, 30 parts of triphenyl phosphate, 8 parts of epoxidized soybean oil, 2.5 parts of triethyl phosphoryl acetate, 7 parts of ammonium polyphosphate, 8 parts of molybdenum trioxide, 15 parts of zirconium hydroxide, 10 parts of zinc oxide and 2 parts of lauryl methacrylate.
The flame retardant consists of the following raw materials in parts by weight: 22 parts of zinc borate, 18 parts of zinc oxide, 15 parts of zinc dihydrogen phosphate, 15 parts of aluminum hydroxide, 7 parts of magnesium chloride, 10 parts of diatomite and 4 parts of ammonium polyphosphate.
The light-storing ink consists of the following raw materials in parts by weight: 22 parts of white ink, 15 parts of acrylic resin, 6 parts of methyl isobutyl ketone, 10 parts of diethylene glycol ethyl ether, 3 parts of trimethyl hexamethylene diamine, 4 parts of flame retardant and 32 parts of light-storing liquid, wherein the light-storing liquid is prepared by mixing zinc sulfide, varnish and ethanol according to the weight ratio of 10:10: 3.
The back glue layer comprises the following raw materials in parts by weight: 65 parts of water-based acrylic resin, 22 parts of clam meal, 4 parts of polypropylene glycol, 0.4 part of flatting agent, 0.4 part of defoaming agent and 25 parts of deionized water.
The preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 90s at 75 ℃ to form a light-storing layer;
coating shading slurry on the bottom surface of the light storage layer, and drying at 65 ℃ to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 55 ℃ for 95s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying at 65 ℃, and compounding with the shading layer at the temperature of 100 ℃ for 25s to form the flame-retardant light-storing film.
Specifically, the preparation method of the light-storing ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at the normal temperature and the rotating speed of 1500r/min for 65 min; and then, continuously adding light storage liquid and a flame retardant, and stirring at the rotating speed of 1500r/min for 55min to obtain the light storage ink.
In the first step, the coating thickness of the light-storing ink is 2 filaments.
The light-emitting film obtained in example 3 was subjected to flame retardancy test according to UL94, and after two 10-second burning tests, the flame was extinguished within 10 seconds, and no burning material was dropped, and the flame retardancy rating reached V-0 rating.
The transparent flame-retardant protective layer is added with triphenyl phosphate to be cooperatively matched with ammonium polyphosphate, molybdenum trioxide, zirconium oxide and zinc oxide, so that the smoke generation amount of the finally formed light-storing film is reduced by 50-80%, the oxygen index is improved by 40-55%, the effect of self-extinguishing after leaving fire is achieved, the flame-retardant property is detected according to UL94, and the flame-retardant grade of the light-storing film can reach V-0 level; the epoxy soybean oil is cooperatively matched with other components, so that the transparent flame-retardant protective layer has excellent heat resistance, and the service life of the light-storing film is ensured; meanwhile, triphenyl phosphate is matched with triethyl phosphoryl acetate, so that PET can be prevented from being degraded, the use of the light storage film is prolonged, and the light storage film also has a certain antioxidation effect, and the protective layer is prevented from being degraded and discolored.
The flame retardant in the light storage ink can improve the oxygen index of a light storage layer by 10-20% by matching zinc borate, zinc oxide, zinc dihydrogen phosphate, aluminum hydroxide, magnesium chloride, diatomite and ammonium polyphosphate so as to improve the flame retardant property of a light storage film.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents and modifications within the scope of the description.
Claims (8)
1. The preparation method of the flame-retardant light-storing film is characterized by comprising the following steps: the light-storing film comprises a transparent flame-retardant protective layer, a light-storing layer, a light-shielding layer, a back adhesive layer and a release paper layer, wherein the transparent flame-retardant protective layer comprises the following raw materials in parts by weight: PET90-110 parts, triphenyl phosphate 25-35 parts, epoxidized soybean oil 5-10 parts, triethyl phosphonoacetate 2-3 parts, ammonium polyphosphate 5-10 parts, molybdenum trioxide 6-10 parts, zirconium hydroxide 12-18 parts, zinc oxide 8-12 parts, and lauryl methacrylate 1-3 parts;
the preparation method comprises the following steps:
coating light-storing ink on the surface of a PMMA film, and drying for 80-100s at 70-80 ℃ to form a light-storing layer;
step two, coating shading slurry on the bottom surface of the light storage layer, and drying to form a shading layer;
coating transparent flame-retardant slurry on the top surface of the light-storing layer, and drying at 50-60 ℃ for 90-100s to form a transparent flame-retardant protective layer;
and step four, coating the back adhesive slurry on the release paper, drying and compounding with the shading layer to form the flame-retardant light storage film.
2. The method for producing a flame-retardant light-storing film according to claim 1, characterized in that: the light-storing ink is prepared from the following raw materials in parts by weight: 18-25 parts of white ink, 12-18 parts of acrylic resin, 5-8 parts of methyl isobutyl ketone, 8-12 parts of diethylene glycol ethyl ether, 2-4 parts of trimethyl hexamethylene diamine, 3-5 parts of a flame retardant and 30-35 parts of a light-storing liquid.
3. The method for producing a flame-retardant light-storing film according to claim 2, characterized in that: the flame retardant consists of the following raw materials in parts by weight: 20-25 parts of zinc borate, 15-22 parts of zinc oxide, 10-18 parts of zinc dihydrogen phosphate, 10-20 parts of aluminum hydroxide, 5-10 parts of magnesium chloride, 8-12 parts of kieselguhr and 3-5 parts of ammonium polyphosphate.
4. The method for producing a flame-retardant light-storing film according to claim 2, characterized in that: the light storage liquid is formed by mixing zinc sulfide, varnish and ethanol according to the weight ratio of 10:10: 3.
5. The method for producing a flame-retardant light-storing film according to claim 1, characterized in that: the back glue layer comprises the following raw materials in parts by weight: 60-70 parts of water-based acrylic resin, 20-25 parts of clam powder, 3-5 parts of polypropylene glycol, 0.3-0.5 part of flatting agent, 0.2-0.5 part of defoaming agent and 20-30 parts of deionized water.
6. The method for producing a flame-retardant light-storing film according to claim 1, characterized in that: the preparation method of the light-storing ink comprises the following steps: adding white ink, acrylic resin, methyl isobutyl ketone, diethylene glycol ethyl ether and trimethyl hexamethylene diamine into a container, and stirring at the normal temperature and the rotating speed of 1000-2000r/min for 60-70 min; and then, continuously adding the light storage liquid and the flame retardant, and stirring for 50-60min at the rotating speed of 1000-2000r/min to obtain the light storage ink.
7. The method for producing a flame-retardant light-storing film according to claim 1, characterized in that: in the first step, the coating thickness of the light-storing ink is 1-2 filaments.
8. The method for producing a flame-retardant light-storing film according to claim 1, characterized in that: in the fourth step, the composite environment of the back adhesive layer and the shading layer is as follows: the temperature is 90-110 ℃ and the time is 20-30 s.
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CN110033716A (en) * | 2019-04-26 | 2019-07-19 | 泉州市夜景辉反光材料有限公司 | A kind of light storage film and preparation method thereof |
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CN102173165A (en) * | 2011-03-14 | 2011-09-07 | 曹其焕 | Light-storing luminous anti-counterfeiting film, and manufacturing method and application thereof |
JP2013139106A (en) * | 2012-01-04 | 2013-07-18 | Hiraoka & Co Ltd | White light storage luminescence film material |
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