CN103205223B - A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application - Google Patents

A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application Download PDF

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CN103205223B
CN103205223B CN201210312006.3A CN201210312006A CN103205223B CN 103205223 B CN103205223 B CN 103205223B CN 201210312006 A CN201210312006 A CN 201210312006A CN 103205223 B CN103205223 B CN 103205223B
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protection film
sensitive
emulsion
component
temperature
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CN103205223A (en
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冯小平
李胜华
姜云刚
何伟
武鹏
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Hubei Institute of Aerospace Chemical Technology
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Hubei Institute of Aerospace Chemical Technology
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Abstract

A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application.Surface protection film single component emulsion pressure-sensitive of the present invention is the polyacrylate dispersion that butyl acrylate, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) adopt the synthesis of pre-emulsification semi-continuous polymerzation technique.Solve the deficiency that the existing palpus of protective membrane pressure sensitive adhesive in the art additional crosslink agent could use; the surface protection film stripping strength made of surface protection film single component emulsion pressure-sensitive of the present invention is moderate; good to PVC profile, aluminum oxide section bar and appliance plate attaching property; without cull and fleck after peeling off, do not pollute PVC profile, aluminum oxide section bar and appliance plate.

Description

A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application
Technical field
The present invention relates to a kind of surface protection film single component emulsion pressure-sensitive, and the application on electric protection film of being in, PVC profile protective membrane and aluminum oxide section bar protective membrane.
Background technology
Along with the fast development of national economy, the use in productive life of architectural shape and household appliances is more and more wider.PVC profile for building and aluminum oxide section bar and household appliances, in production, storage and transportation, need to protect its outside surface, to prevent the corrosion of obnoxious flavour, microorganism, dust pollution, or avoid machinery to scratch producing scratch etc.One of method the most often used is now on the surface of protected object, the layer protecting film (i.e. surface protection film) sticked, and after the process such as end transport, storage, processing and assembling, then throws off this film.
PVC profile for building and aluminum oxide section bar and the existing market of household appliances surface protection film adopt bicomponent latex of polyacrylate pressure sensitive adhesive usually, regulates stripping strength by the method for additional crosslink agent, improve cohesive strength.Additional crosslink agent not only increases production process, and owing to being usually less than 10 hours the working life of emulsion pressure-sensitive after adding linking agent, prepares pressure sensitive adhesive residual in the pressure sensitive adhesive and glue groove do not used and not only causes waste and to environment.And single component pressure sensitive adhesive can avoid the problems referred to above, and use easily.
Summary of the invention
One is the object of the present invention is to provide to have well attaching property to PVC profile, aluminum oxide section bar and appliance plate; do not pollute PVC profile, aluminum oxide section bar and appliance plate after stripping, can be used for the single component emulsion pressure-sensitive of the surface protection of PVC profile, aluminum oxide section bar and appliance plate.
The present invention also aims to its preparation method that above-mentioned single component emulsion pressure-sensitive is provided.
The present invention also aims to provide above-mentioned single component emulsion pressure-sensitive to the application in the surface protection of PVC profile, aluminum oxide section bar and appliance plate.
Acrylate emulsion cohesive strength is usually not high, and high-temp resisting high-humidity resisting aging resistance is poor, can not be directly used in the making of protective membrane, and therefore, synthetic surface protective membrane pressure sensitive adhesive key is exactly improve the cohesive strength of pressure sensitive adhesive.
In the present invention, apart from outside explanation, the ratio adopted is weight ratio.
Object of the present invention is reached by following scheme:
Surface protection film single component emulsion pressure-sensitive of the present invention is the polyacrylate dispersion adopting the synthesis of pre-emulsification semi-continuous polymerzation technique containing butyl acrylate, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA).
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is as follows by weight:
Butyl acrylate 38.0 ~ 40.5
Vinyl acetate 1.8 ~ 3.6
Vinylformic acid 0.9 ~ 1.8
N hydroxymethyl acrylamide 0.5 ~ 0.8
Allyl methacrylate(AMA) 0.5 ~ 0.9
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2 ~ 0.4
Ammonium persulphate 0.1 ~ 0.2
Sodium bicarbonate 0.1 ~ 0.2
Neutralizing agent 0.2 ~ 0.4
Deionized water 53.8 ~ 54.3.
Optimum ratio of the present invention is by weight:
Butyl acrylate 39.5 ~ 40.0
Vinyl acetate 2.7 ~ 3.5
Vinylformic acid 0.9 ~ 1.3
N hydroxymethyl acrylamide 0.5 ~ 0.6
Allyl methacrylate(AMA) 0.5 ~ 0.6
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2 ~ 0.3
Ammonium persulphate 0.13 ~ 0.18
Sodium bicarbonate 0.1 ~ 0.12
Neutralizing agent 0.2 ~ 0.3
Deionized water 53.8 ~ 54.3.
Neutralizing agent of the present invention is dimethylethanolamine or concentration is the ammoniacal liquor of 25%.
The step of surface protection film single component emulsion pressure-sensitive preparation method of the present invention is as follows:
(1) by 40% ~ 60% of deionized water gross weight, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate gross weight 50% ~ 100%, 50% ~ 75% and butyl acrylate of ammonium persulphate gross weight, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to add in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) sodium bicarbonates whole to remaining deionized water (40% ~ 60% of the gross weight that feeds intake), disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate (0 ~ 50% of the gross weight that feeds intake), ammonium persulphate (25 ~ 50% of the gross weight that feeds intake) and charging capacity is dropped in reactor, be warming up to 80 ± 1 DEG C, add the gross weight 5% ~ 12% of pre-emulsion, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion (gross weight 88 ~ 95%) is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises, and temperature of reaction is raised to 90 DEG C, keeps temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature, when temperature of reaction kettle is lower than 40 DEG C, add neutralizing agent; filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Surface protection film single component emulsion pressure-sensitive of the present invention can directly carry out upper machine coating, with surface protection film single component emulsion pressure-sensitive of the present invention without the need to additional crosslink agent, can save and join glue process, eliminate simultaneously and join glue mistake, also cost-saved and residue reduces the pollution to environment; The surface protection film stripping strength made is moderate, good to PVC profile, aluminum oxide section bar and appliance plate attaching property, and has good high-temp resisting high-humidity resisting aging resistance, without cull and fleck after peeling off, does not pollute PVC profile, aluminum oxide section bar and appliance plate.
Embodiment
Embodiment 1
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Butyl acrylate 40.5
Vinyl acetate 2.2
Vinylformic acid 0.9
N hydroxymethyl acrylamide 0.5
Allyl methacrylate(AMA) 0.9
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2
Ammonium persulphate 0.2
Sodium bicarbonate 0.1
Dimethylethanolamine 0.2
Deionized water 54.3.
The concrete steps of the preparation method of surface protection film single component emulsion pressure-sensitive of the present invention are as follows:
(1) deionized water of 60%, the ammonium persulphate of 75% and whole disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates, butyl acrylate, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to be added in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the pre-emulsion of 5%, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises, and temperature of reaction is raised to 90 DEG C, keeps temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature, when temperature of reaction kettle is lower than 40 DEG C, add dimethylethanolamine; filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Protective membrane performance is: stripping strength (0.6N/25mm); High-temp resisting high-humidity resisting (65 DEG C, 80%RH aging 72h does not fall glue).Be applicable to the surface protection of aluminum oxide section bar and appliance plate.
Embodiment 2
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Butyl acrylate 40.1
Vinyl acetate 1.8
Vinylformic acid 1.8
N hydroxymethyl acrylamide 0.8
Allyl methacrylate(AMA) 0.5
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.4
Ammonium persulphate 0.15
Sodium bicarbonate 0.2
The ammoniacal liquor 0.35 of concentration 25%
Deionized water 53.9
The concrete steps of the preparation method of surface protection film single component emulsion pressure-sensitive of the present invention are as follows:
(1) deionized water of 50%, the disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate of 50%, the ammonium persulphate of 67% and whole butyl acrylates, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to be added in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the pre-emulsion of 12%, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises; temperature of reaction is raised to 90 DEG C; keep temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature; when temperature of reaction kettle is lower than 40 DEG C; add the ammoniacal liquor of concentration 25%, filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Protective membrane performance is: stripping strength (0.6N/25mm); High-temp resisting high-humidity resisting (65 DEG C, 80%RH aging 72h does not fall glue).Be applicable to the surface protection of PVC profile and aluminum oxide section bar.
Embodiment 3
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Butyl acrylate 38.3
Vinyl acetate 3.6
Vinylformic acid 1.8
N hydroxymethyl acrylamide 0.8
Allyl methacrylate(AMA) 0.5
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.3
Ammonium persulphate 0.1
Sodium bicarbonate 0.2
The ammoniacal liquor 0.4 of concentration 25%
Deionized water 54.0.
The concrete steps of the preparation method of surface protection film single component emulsion pressure-sensitive of the present invention are as follows:
(1) deionized water of 60%, the disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate of 75%, the ammonium persulphate of 50% and whole butyl acrylates, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to be added in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the pre-emulsion of 10%, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises; temperature of reaction is raised to 90 DEG C; keep temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature; when temperature of reaction kettle is lower than 40 DEG C; add the ammoniacal liquor of concentration 25%, filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Protective membrane performance: stripping strength (0.7N/25mm); Wet and heat ageing resistant performance (65 DEG C, 80%RH aging 72h does not fall glue); Be applicable to the surface protection of PVC profile and aluminum oxide section bar.
Embodiment 4
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Butyl acrylate 38.7
Vinyl acetate 3.6
Vinylformic acid 1.3
N hydroxymethyl acrylamide 0.6
Allyl methacrylate(AMA) 0.8
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2
Ammonium persulphate 0.2
Sodium bicarbonate 0.1
Dimethylethanolamine 0.3
Deionized water 54.2.
The concrete steps of the preparation method of surface protection film single component emulsion pressure-sensitive of the present invention are as follows:
(1) deionized water of 40%, the ammonium persulphate of 75% and whole disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates, butyl acrylate, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to be added in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the pre-emulsion of 6%, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises, and temperature of reaction is raised to 90 DEG C, keeps temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature, when temperature of reaction kettle is lower than 40 DEG C, add dimethylethanolamine; filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Protective membrane performance: stripping strength (0.5N/25mm); Wet and heat ageing resistant performance (65 DEG C, 80%RH aging 72h does not fall glue); Be applicable to the surface protection of appliance plate.
Embodiment 5
Surface protection film single component emulsion pressure-sensitive of the present invention is polymerized in a kettle. by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Butyl acrylate 38.0
Vinyl acetate 3.5
Vinylformic acid 1.8
N hydroxymethyl acrylamide 0.8
Allyl methacrylate(AMA) 0.9
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.4
Ammonium persulphate 0.2
Sodium bicarbonate 0.2
The ammoniacal liquor 0.4 of concentration 25%
Deionized water 53.8.
The concrete steps of the preparation method of surface protection film single component emulsion pressure-sensitive of the present invention are as follows:
(1) obtain deionized water, the disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate of 50%, the ammonium persulphate of 75% and whole butyl acrylates, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) by 40% and to add in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the pre-emulsion of 10%, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises; temperature of reaction is raised to 90 DEG C; keep temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature; when temperature of reaction kettle is lower than 40 DEG C; add the ammoniacal liquor of concentration 25%, filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
Protective membrane performance: stripping strength (0.8N/25mm); Wet and heat ageing resistant performance (65 DEG C, 80%RH aging 72h does not fall glue); Be applicable to the surface protection of PVC profile and aluminum oxide section bar.

Claims (4)

1. a surface protection film single component emulsion pressure-sensitive, is characterized in that the polyacrylate dispersion for adopting the synthesis of pre-emulsification semi-continuous polymerzation technique containing butyl acrylate, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA); Be polymerized in a kettle. by following component raw material and prepare, its composition and ratio is as follows by weight:
Butyl acrylate 38.0 ~ 40.5
Vinyl acetate 1.8 ~ 3.6
Vinylformic acid 0.9 ~ 1.8
N hydroxymethyl acrylamide 0.5 ~ 0.8
Allyl methacrylate(AMA) 0.5 ~ 0.9
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2 ~ 0.4
Ammonium persulphate 0.1 ~ 0.2
Sodium bicarbonate 0.1 ~ 0.2
Neutralizing agent 0.2 ~ 0.4
Deionized water 53.8 ~ 54.3;
Comprise the steps:
(1) by 40% ~ 60% of deionized water gross weight, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate gross weight 50% ~ 100%, 50% ~ 75% and butyl acrylate of ammonium persulphate gross weight, vinyl acetate, vinylformic acid, N hydroxymethyl acrylamide and allyl methacrylate(AMA) to add in emulsifying kettle emulsification 25 ~ 30 minutes, obtained pre-emulsion;
(2) remaining deionized water, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, ammonium persulphate and whole sodium bicarbonates are dropped in reactor, be warming up to 80 ± 1 DEG C, add the gross weight 5% ~ 12% of pre-emulsion, still temperature rise reacts 30 ~ 40 minutes again after the highest, then remaining pre-emulsion is dripped, pre-emulsion dropwised in about 4 hours, kept still temperature at 80 ± 2 DEG C in dropping process;
(3) pre-emulsion dropwises, and temperature of reaction is raised to 90 DEG C, keeps temperature of reaction 89 DEG C ~ 91 DEG C reactions 1 hour; then lower the temperature, when temperature of reaction kettle is lower than 40 DEG C, add neutralizing agent; filter discharging with 300 mesh filter screens, obtain surface protection film single component emulsion pressure-sensitive.
2. surface protection film single component emulsion pressure-sensitive according to claim 1, is characterized in that: be polymerized in a kettle. by following component raw material and prepare, its composition and ratio is counted as follows by weight:
Butyl acrylate 39.5 ~ 40.0
Vinyl acetate 2.7 ~ 3.5
Vinylformic acid 0.9 ~ 1.3
N hydroxymethyl acrylamide 0.5 ~ 0.6
Allyl methacrylate(AMA) 0.5 ~ 0.6
Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 0.2 ~ 0.3
Ammonium persulphate 0.13 ~ 0.18
Sodium bicarbonate 0.1 ~ 0.12
Neutralizing agent 0.2 ~ 0.3
Deionized water 53.8 ~ 54.3.
3. surface protection film single component emulsion pressure-sensitive according to claim 1 or 2, is characterized in that: described neutralizing agent is dimethylethanolamine or concentration is the ammoniacal liquor of 25%.
4. the application of single component emulsion pressure-sensitive in the surface protection film of appliance plate, PVC profile and aluminum oxide section bar of surface protection film described in a claim 1 or 2.
CN201210312006.3A 2012-08-29 2012-08-29 A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application Active CN103205223B (en)

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CN104371607B (en) * 2013-08-12 2016-08-17 湖北航天化学技术研究所 High-solid-content and low-viscosity acrylate emulsion stick and preparation method
CN105315924B (en) * 2014-07-22 2017-11-07 湖北航天化学技术研究所 A kind of micro- viscous emulsion pressure-sensitive and preparation method thereof
CN108285508B (en) * 2017-01-20 2020-10-30 湖北航天化学技术研究所 Medium-high viscosity emulsion type acrylate pressure-sensitive adhesive for protective film, and preparation method and application thereof
US20200377763A1 (en) * 2017-12-27 2020-12-03 Lg Chem, Ltd. Adhesive Composition and Protective Film Produced Using Same
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