CN117624695A - Window protection film for decoration protection and preparation method thereof - Google Patents

Window protection film for decoration protection and preparation method thereof Download PDF

Info

Publication number
CN117624695A
CN117624695A CN202410102324.XA CN202410102324A CN117624695A CN 117624695 A CN117624695 A CN 117624695A CN 202410102324 A CN202410102324 A CN 202410102324A CN 117624695 A CN117624695 A CN 117624695A
Authority
CN
China
Prior art keywords
weight
parts
stirring
film
asa
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202410102324.XA
Other languages
Chinese (zh)
Inventor
孙强云
邓迎春
高晓梅
姜嘉林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Haiyang Linghui Packaging Co ltd
Original Assignee
Haiyang Linghui Packaging Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Haiyang Linghui Packaging Co ltd filed Critical Haiyang Linghui Packaging Co ltd
Priority to CN202410102324.XA priority Critical patent/CN117624695A/en
Publication of CN117624695A publication Critical patent/CN117624695A/en
Pending legal-status Critical Current

Links

Abstract

The invention relates to the technical field of protective films, in particular to a window protective film for decoration and a preparation method thereof, wherein butyl acrylate, styrene and acrylonitrile are used as raw materials, self-made ASA resin powder prepared by a seed emulsion polymerization method has better weather resistance, mechanical properties can not be obviously reduced after long-term exposure to outdoor environment, and a film prepared by blending the self-made ASA resin powder with titanium dioxide with modified surfaces has better ultraviolet absorption capacity, so that the prepared ASA film has better ultraviolet resistance on the basis of better mechanical properties; and secondly, the organosilicon coating component prepared by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials has better wear resistance, and the wear resistance of the ASA film can be enhanced by coating the organosilicon coating component on the surface of the ASA film.

Description

Window protection film for decoration protection and preparation method thereof
Technical Field
The invention relates to the technical field of protective films, in particular to a window protective film for decoration protection and a preparation method thereof.
Background
At present, window protection films are widely used in the finishing process, and the main purpose of the window protection films is to prevent dust, dirt and scratches from polluting and damaging the window surface in the finishing process. Most of traditional window protection films are plastic films, and have certain protection effects, but have more problems such as poor ultraviolet resistance, easy aging and color change after long-time exposure to sunlight, and influence on attractiveness and service life; lack of sufficient strength and toughness, easy breakage, and inability to effectively resist impact and scratch from external force; the abrasion-resistant effect is poor, and the damage is easy to occur in the decoration construction process. In order to solve the above problems, many protective films having different properties are commercially available, but these protective films have not reached an ideal optimum state in practical use.
The utility model discloses a plastic film for window and preparation method thereof of publication No. CN107163276A, the plastic film includes the PET basic unit, and the one side of PET basic unit has wear-resisting stable layer, and the another side of PET basic unit has light fire-retardant layer, and the surface on wear-resisting stable layer and light fire-retardant layer all has the protection film layer. However, the ultraviolet resistance of the plastic film for windows prepared by the invention is not further improved, so that the plastic film is improved in the technology of the invention, and the prepared protective film can have better wear resistance and ultraviolet resistance at the same time.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention provides a window protection film for decoration protection and a preparation method thereof, which aims to make the window protection film better applicable to the decoration protection industry.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a preparation method of a window protection film for decoration protection comprises the following steps:
step1, preparing self-made ASA resin powder by using butyl acrylate, styrene and acrylonitrile as raw materials through a seed emulsion polymerization method;
step2, carrying out surface modification on nano titanium dioxide by gamma- (2, 3-glycidoxy) propyl trimethoxy silane to obtain modified titanium dioxide;
step3, weighing 58-65 parts by weight of self-made ASA resin powder and 4-5 parts by weight of modified titanium dioxide, pouring the self-made ASA resin powder and the modified titanium dioxide into a high-speed mixer for blending, heating and extruding the mixture into a film by a double-screw extruder after blending, and cooling the film by a cooling roller to obtain an ASA film;
step4, preparing an organosilicon coating component by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials;
step5, rolling the organosilicon coating component on the surface of the ASA film, placing the ASA film in a baking oven at 50 ℃ for 5-6min, and then placing the ASA film in a baking oven at 70 ℃ for 25-30min to obtain the window protection film for decoration and protection.
Further, the preparation steps of the self-made ASA resin powder in Step1 are as follows:
1, weighing 1-2 parts by weight of sodium dodecyl sulfate and 2-3 parts by weight of potassium persulfate, pouring the sodium dodecyl sulfate and the potassium persulfate into a flask filled with 200 parts by weight of deionized water, stirring until the sodium dodecyl sulfate and the potassium persulfate are dissolved, adding 33-35 parts by weight of butyl acrylate and 2-3 parts by weight of allyl methacrylate, introducing nitrogen for protection, heating to 70 ℃, and reacting for 3 hours at constant temperature under stirring conditions, wherein the obtained mixture is marked as a seed system;
step2, weighing 95-100 parts by weight of seed system, adding 1-2 parts by weight of cumene hydroperoxide, uniformly mixing to obtain a first system, weighing 100 parts by weight of seed system, adding 38-45 parts by weight of deionized water, 0.3-0.4 part by weight of sodium dodecyl sulfate and 0.2-0.3 part by weight of potassium persulfate, uniformly mixing again, adding 2-3 parts by weight of sodium formaldehyde sulfoxylate aqueous solution, heating to 70 ℃, and dropwise adding the first system to obtain a mixed system;
step3, weighing 45-46 parts by weight of styrene, 15-16 parts by weight of acrylonitrile, 1-2 parts by weight of cumene hydroperoxide and 0.1-0.2 part by weight of sodium dodecyl sulfate, mixing uniformly, marking the mixture as a monomer component, dripping the monomer component into a mixed system heated to 70 ℃, and performing heat preservation reaction for 35-40min to obtain an ASA mixed system;
and 4, adding 5-6% of magnesium sulfate aqueous solution into the ASA mixed system, stirring for 15-20min, performing suction filtration, washing with deionized water, and drying to obtain the self-made ASA resin powder.
Further, the stirring speed of stirring until dissolution in the step1 is 100-200r/min, the stirring time of stirring until dissolution is 8-10min, and the stirring speed of stirring conditions in the step1 is 200r/min.
Further, the stirring speed of the uniform mixing in the step2 is 200-300r/min, the stirring time of the uniform mixing is 8-10min, the stirring speed of the uniform mixing in the step2 is 100-200r/min, the stirring time of the uniform mixing again is 12-15min, the concentration of the sodium formaldehyde sulfoxylate aqueous solution in the step2 is 0.25mg/L, and the dropping speed in the step2 is 1-2 drops/s.
Further, the stirring speed of the full mixing in the step3 is 100-200r/min, the stirring time of the full mixing is 12-15min, and the dripping speed in the step3 is 1-2 drops/s.
Further, the mass concentration of the magnesium sulfate aqueous solution in the step4 is 10%, the stirring speed in the step4 is 100-200r/min, the drying temperature in the step4 is 70 ℃, and the drying time is 24h.
Further, the preparation method of the modified titanium dioxide in Step2 comprises the following steps:
step A, absolute ethyl alcohol and glacial acetic acid are mixed according to a ratio of 3:1, stirring for 3-5min at a stirring speed of 300-500r/min, dripping tetrabutyl titanate with 5-8% of the weight of the tetrabutyl titanate, and stirring for 30min at a stirring speed of 800-1000r/min under a water bath condition at 30 ℃ to obtain a component to be reacted;
step B, adjusting the pH value of a component to be reacted to 1 by using hydrochloric acid with the concentration of 1mol/L, then dripping ethanol aqueous solution with the mass concentration of 60% and the weight of 35-40% into the component at the dripping speed of 1 drop/s, heating the solution to 70 ℃ and then reacting for 12 hours to obtain the titanium dioxide sol;
and C, weighing 8-10 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, dispersing into 100 parts by weight of absolute ethyl alcohol, heating to 70 ℃, dripping 25-30 parts by weight of titanium dioxide sol at a dripping speed of 1 drop/s, reacting for 12 hours, drying in a drying oven at 65 ℃, grinding, and sieving with a 200-mesh sieve to obtain the modified titanium dioxide.
Further, the preparation steps of the organosilicon coating component in Step4 are as follows:
step one, weighing 28-30 parts by weight of tetraethoxysilane, 14-15 parts by weight of phenyl trimethoxysilane, 3-4 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 2-3 parts by weight of dimethyl dimethoxy silane, mixing and stirring uniformly to obtain a first component, weighing 22-25 parts by weight of isopropanol, 22-23 parts by weight of deionized water and 0.3-0.4 part of glacial acetic acid, mixing and stirring uniformly to obtain a second component;
and step two, dropwise adding the first component into the second component under the condition of stirring, heating the second component to 60 ℃ in a water bath after the dropwise adding, and preserving the heat for 8 hours to obtain the organosilicon coating component.
Further, the stirring speed of the uniform mixing and stirring in the first step is 100-200r/min, the stirring time of the uniform mixing and stirring is 8-10min, and the dripping speed in the second step is 1-2 drops/s.
A window protection film for decoration protection, the composition of the window protection film for decoration protection comprising: butyl acrylate, styrene, acrylonitrile, sodium lauryl sulfate, potassium persulfate, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, tetrabutyl titanate, ethyl orthosilicate, phenyl trimethoxysilane and dimethyl dimethoxy silane.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes butyl acrylate, styrene and acrylonitrile as raw materials, the self-made ASA resin powder prepared by a seed emulsion polymerization method has better weather resistance, mechanical properties can not be obviously reduced after long-term exposure to outdoor environment, and a film prepared by blending the self-made ASA resin powder with titanium dioxide with modified surfaces has better ultraviolet absorption capacity, so that the prepared ASA film has better ultraviolet resistance on the basis of better mechanical properties; and secondly, the organosilicon coating component prepared by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials has better wear resistance, and the surface of the ASA film can be coated with the organosilicon coating component to enhance the wear resistance of the ASA film, so that the prepared window protection film for decoration has higher hardness and wear resistance grade, and can be better applied to the decoration protection industry.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further described below with reference to examples.
Example 1
The preparation method of the window protection film for decoration protection in the embodiment comprises the following steps:
step1, preparing self-made ASA resin powder by using butyl acrylate, styrene and acrylonitrile as raw materials through a seed emulsion polymerization method;
the preparation method of the self-made ASA resin powder in Step1 comprises the following steps:
1, weighing 1 part by weight of sodium dodecyl sulfate and 2 parts by weight of potassium persulfate, pouring the mixture into a flask filled with 200 parts by weight of deionized water, stirring until the mixture is dissolved, adding 33 parts by weight of butyl acrylate and 2 parts by weight of allyl methacrylate, introducing nitrogen for protection, heating to 70 ℃, reacting for 3 hours at constant temperature under stirring conditions, and stirring the mixture to obtain a seed system, wherein the stirring speed of stirring until the mixture is dissolved is 100r/min, the stirring time of stirring until the mixture is dissolved is 8min, and the stirring speed of stirring under stirring conditions is 200r/min;
step2, weighing 95 parts by weight of seed system, adding 1 part by weight of cumene hydroperoxide, uniformly mixing to obtain a first system, weighing 100 parts by weight of seed system, adding 38 parts by weight of deionized water, 0.3 part by weight of sodium dodecyl sulfate and 0.2 part by weight of potassium persulfate, uniformly mixing again, adding 2 parts by weight of sodium formaldehyde sulfoxylate aqueous solution, heating to 70 ℃, dropwise adding the first system, obtaining a mixed system, uniformly mixing at a stirring speed of 200r/min, uniformly mixing for 8min, uniformly mixing again for a stirring speed of 100r/min, uniformly mixing again for 12min, and dropwise adding the sodium formaldehyde sulfoxylate aqueous solution at a concentration of 0.25mg/L at a dripping speed of 1 drop/s;
step3, weighing 45 parts by weight of styrene, 15 parts by weight of acrylonitrile, 1 part by weight of cumene hydroperoxide and 0.1 part by weight of sodium dodecyl sulfate, mixing the components uniformly, marking the components as monomer components, dropwise adding the monomer components into a mixed system heated to 70 ℃, carrying out heat preservation reaction for 35min, marking the components as an ASA mixed system, stirring the components uniformly at a stirring speed of 100r/min, and stirring the components uniformly for 12min at a dripping speed of 1 drop/s;
and 4, adding 5% of magnesium sulfate aqueous solution into the ASA mixed system, stirring for 15min, performing suction filtration, washing with deionized water, and drying to obtain the self-made ASA resin powder, wherein the mass concentration of the magnesium sulfate aqueous solution is 10%, the stirring speed is 100r/min, the drying temperature is 70 ℃, and the drying time is 24h.
Step2, carrying out surface modification on nano titanium dioxide by gamma- (2, 3-glycidoxy) propyl trimethoxy silane to obtain modified titanium dioxide;
wherein, the preparation steps of the modified titanium dioxide in Step2 comprise:
step A, absolute ethyl alcohol and glacial acetic acid are mixed according to a ratio of 3:1, stirring for 3min at a stirring speed of 300r/min, then dripping tetrabutyl titanate with 5% of the weight of the tetrabutyl titanate, and stirring for 30min at a stirring speed of 800r/min under a water bath condition at 30 ℃, wherein the obtained mixture is marked as a component to be reacted;
step B, adjusting the pH value of a component to be reacted to 1 by using hydrochloric acid with the concentration of 1mol/L, then dripping ethanol aqueous solution with the mass concentration of 60% and the weight of 35% at the dripping speed of 1 drop/s, heating to 70 ℃ and reacting for 12 hours to obtain the titanium dioxide sol;
and C, weighing 8 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, dispersing into 100 parts by weight of absolute ethyl alcohol, heating to 70 ℃, dripping 25 parts by weight of titanium dioxide sol at a dripping speed of 1 drop/s, reacting for 12 hours, drying in a drying oven at 65 ℃, grinding, and sieving with a 200-mesh sieve to obtain the modified titanium dioxide.
Step3, weighing 58 parts by weight of self-made ASA resin powder and 4 parts by weight of modified titanium dioxide, pouring the self-made ASA resin powder and the modified titanium dioxide into a high-speed mixer for blending, heating and extruding the mixture into a film by a double-screw extruder after blending, and cooling the film by a cooling roller to obtain an ASA film;
step4, preparing an organosilicon coating component by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials;
the preparation method of the organosilicon coating component in Step4 comprises the following steps:
step one, weighing 28 parts by weight of tetraethoxysilane, 14 parts by weight of phenyl trimethoxysilane, 3 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 2 parts by weight of dimethyl dimethoxy silane, uniformly mixing and stirring to obtain a first component, weighing 22 parts by weight of isopropanol, 22 parts by weight of deionized water and 0.3 glacial acetic acid, uniformly mixing and stirring to obtain a second component, wherein the stirring speed of uniform mixing and stirring is 100r/min, and the stirring time of uniform mixing and stirring is 8min;
and step two, dropwise adding the first component into the second component under the condition of stirring, heating the second component to 60 ℃ in a water bath after the dropwise adding, and preserving heat for 8 hours to obtain the organosilicon coating component, wherein the dropwise adding speed is 1 drop/s.
Step5, rolling the organosilicon coating component on the surface of the ASA film, placing the ASA film in a baking oven at 50 ℃ for 5min, and then placing the ASA film in a baking oven at 70 ℃ for 25min to obtain the window protection film for decoration protection.
A window protection film for decoration protection comprises the following components: butyl acrylate, styrene, acrylonitrile, sodium lauryl sulfate, potassium persulfate, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, tetrabutyl titanate, ethyl orthosilicate, phenyl trimethoxysilane and dimethyl dimethoxy silane.
Example 2
The preparation method of the window protection film for decoration protection in the embodiment comprises the following steps:
step1, preparing self-made ASA resin powder by using butyl acrylate, styrene and acrylonitrile as raw materials through a seed emulsion polymerization method;
the preparation method of the self-made ASA resin powder in Step1 comprises the following steps:
step1, weighing 2 parts by weight of sodium dodecyl sulfate and 3 parts by weight of potassium persulfate, pouring the materials into a flask filled with 200 parts by weight of deionized water, stirring until the materials are dissolved, adding 35 parts by weight of butyl acrylate and 3 parts by weight of allyl methacrylate, introducing nitrogen for protection, heating to 70 ℃, reacting for 3 hours at constant temperature under stirring conditions, and stirring the obtained seed system until the stirring speed of the solution is 200r/min, the stirring time of the stirring until the solution is 10min, and the stirring speed of the stirring conditions is 200r/min;
step2, weighing 100 parts by weight of seed system, adding 2 parts by weight of cumene hydroperoxide, uniformly mixing to obtain a first system, weighing 100 parts by weight of seed system, adding 45 parts by weight of deionized water, 0.4 part by weight of sodium dodecyl sulfate and 0.3 part by weight of potassium persulfate, uniformly mixing again, adding 3 parts by weight of sodium formaldehyde sulfoxylate aqueous solution, heating to 70 ℃, dropwise adding the first system, obtaining a mixed system, uniformly mixing at a stirring speed of 300r/min, uniformly mixing for 10min, uniformly mixing again at a stirring speed of 200r/min, uniformly mixing again for 15min, wherein the concentration of the sodium formaldehyde sulfoxylate aqueous solution is 0.25mg/L, and the dripping speed is 2 drops/s;
step3, weighing 46 parts by weight of styrene, 16 parts by weight of acrylonitrile, 2 parts by weight of cumene hydroperoxide and 0.2 part by weight of sodium dodecyl sulfate, mixing the components fully and uniformly, marking the components as monomer components, dropwise adding the monomer components into a mixed system heated to 70 ℃, carrying out heat preservation reaction for 40min, marking the components as an ASA mixed system, and uniformly mixing the components fully and uniformly at a stirring speed of 200r/min, wherein the stirring time of uniform mixing is 15min, and the dripping speed is 2 drops/s;
and 4, adding a magnesium sulfate aqueous solution with the weight of 6% into the ASA mixed system, stirring for 20min, performing suction filtration, washing with deionized water, and drying to obtain the self-made ASA resin powder, wherein the mass concentration of the magnesium sulfate aqueous solution is 10%, the stirring speed is 200r/min, the drying temperature is 70 ℃, and the drying time is 24h.
Step2, carrying out surface modification on nano titanium dioxide by gamma- (2, 3-glycidoxy) propyl trimethoxy silane to obtain modified titanium dioxide;
wherein, the preparation steps of the modified titanium dioxide in Step2 comprise:
step A, absolute ethyl alcohol and glacial acetic acid are mixed according to a ratio of 3:1, stirring for 5min at a stirring speed of 500r/min, then dripping tetrabutyl titanate with the weight of 8% of the tetrabutyl titanate, stirring for 30min at a stirring speed of 1000r/min under the water bath condition of 30 ℃, and obtaining the components to be reacted;
step B, adjusting the pH value of a component to be reacted to 1 by using hydrochloric acid with the concentration of 1mol/L, then dripping ethanol aqueous solution with the mass concentration of 60% and the weight of 40% at the dripping speed of 1 drop/s, heating to 70 ℃ and reacting for 12 hours to obtain the titanium dioxide sol;
and C, weighing 10 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, dispersing into 100 parts by weight of absolute ethyl alcohol, heating to 70 ℃, dripping 30 parts by weight of titanium dioxide sol at a dripping speed of 1 drop/s, reacting for 12 hours, drying in a drying oven at 65 ℃, grinding, and sieving with a 200-mesh sieve to obtain the modified titanium dioxide.
Step3, weighing 65 parts by weight of self-made ASA resin powder and 5 parts by weight of modified titanium dioxide, pouring the powder into a high-speed mixer for blending, heating and extruding the mixture into a film by a double-screw extruder, and cooling the film by a cooling roller to obtain an ASA film;
step4, preparing an organosilicon coating component by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials;
the preparation method of the organosilicon coating component in Step4 comprises the following steps:
step one, weighing 30 parts by weight of tetraethoxysilane, 15 parts by weight of phenyl trimethoxysilane, 4 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 3 parts by weight of dimethyl dimethoxy silane, uniformly mixing and stirring to obtain a first component, weighing 25 parts by weight of isopropanol, 23 parts by weight of deionized water and 0.4 part of glacial acetic acid, uniformly mixing and stirring to obtain a second component, wherein the stirring speed of uniform mixing and stirring is 200r/min, and the stirring time of uniform mixing and stirring is 10min;
and step two, dropwise adding the first component into the second component under the condition of stirring, heating the second component to 60 ℃ in a water bath after the dropwise adding, and preserving heat for 8 hours to obtain the organosilicon coating component, wherein the dropwise adding speed is 2 drops/s.
Step5, rolling the organosilicon coating component on the surface of the ASA film, placing the ASA film in a baking oven at 50 ℃ for 6min, and then placing the ASA film in a baking oven at 70 ℃ for 30min to obtain the window protection film for decoration protection.
A window protection film for decoration protection comprises the following components: butyl acrylate, styrene, acrylonitrile, sodium lauryl sulfate, potassium persulfate, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, tetrabutyl titanate, ethyl orthosilicate, phenyl trimethoxysilane and dimethyl dimethoxy silane.
Example 3
The preparation method of the window protection film for decoration protection in the embodiment comprises the following steps:
step1, preparing self-made ASA resin powder by using butyl acrylate, styrene and acrylonitrile as raw materials through a seed emulsion polymerization method;
the preparation method of the self-made ASA resin powder in Step1 comprises the following steps:
step1, weighing 2 parts by weight of sodium dodecyl sulfate and 2 parts by weight of potassium persulfate, pouring the materials into a flask filled with 200 parts by weight of deionized water, stirring until the materials are dissolved, adding 34 parts by weight of butyl acrylate and 3 parts by weight of allyl methacrylate, introducing nitrogen for protection, heating to 70 ℃, reacting for 3 hours at constant temperature under stirring conditions, and stirring the obtained seed system until the stirring speed of the solution is 200r/min, wherein the stirring time of the stirring until the solution is 9min, and the stirring speed of the stirring conditions is 200r/min;
step2, weighing 98 parts by weight of seed system, adding 2 parts by weight of cumene hydroperoxide, uniformly mixing to obtain a first system, weighing 100 parts by weight of seed system, adding 41 parts by weight of deionized water, 0.4 part by weight of sodium dodecyl sulfate and 0.3 part by weight of potassium persulfate, uniformly mixing again, adding 2 parts by weight of sodium formaldehyde sulfoxylate aqueous solution, heating to 70 ℃, dropwise adding the first system, obtaining a mixed system, uniformly mixing at a stirring speed of 200r/min, uniformly mixing for 9min, uniformly mixing again at a stirring speed of 200r/min, uniformly mixing again for 13min, wherein the concentration of the sodium formaldehyde sulfoxylate aqueous solution is 0.25mg/L, and the dripping speed is 2 drops/s;
step3, weighing 46 parts by weight of styrene, 15 parts by weight of acrylonitrile, 2 parts by weight of cumene hydroperoxide and 0.2 part by weight of sodium dodecyl sulfate, mixing the components fully and uniformly, marking the components as monomer components, dropwise adding the monomer components into a mixed system heated to 70 ℃, carrying out heat preservation reaction for 38min, marking the components as an ASA mixed system, and uniformly mixing the components fully and uniformly at a stirring speed of 200r/min, wherein the stirring time of uniform mixing is 13min, and the dripping speed is 2 drops/s;
and 4, adding a magnesium sulfate aqueous solution with the weight of 6% into the ASA mixed system, stirring for 18min, performing suction filtration, washing with deionized water, and drying to obtain the self-made ASA resin powder, wherein the mass concentration of the magnesium sulfate aqueous solution is 10%, the stirring speed is 100r/min, the drying temperature is 70 ℃, and the drying time is 24h.
Step2, carrying out surface modification on nano titanium dioxide by gamma- (2, 3-glycidoxy) propyl trimethoxy silane to obtain modified titanium dioxide;
wherein, the preparation steps of the modified titanium dioxide in Step2 comprise:
step A, absolute ethyl alcohol and glacial acetic acid are mixed according to a ratio of 3:1, stirring for 4min at a stirring speed of 400r/min, then dripping tetrabutyl titanate with the weight of 7% of tetrabutyl titanate, stirring for 30min at a stirring speed of 900r/min under the water bath condition of 30 ℃, and obtaining the components to be reacted;
step B, adjusting the pH value of a component to be reacted to 1 by using hydrochloric acid with the concentration of 1mol/L, then dripping an ethanol aqueous solution with the mass concentration of 60% and the weight of 38% at the dripping speed of 1 drop/s, heating to 70 ℃ and reacting for 12 hours to obtain the titanium dioxide sol;
and C, weighing 9 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, dispersing into 100 parts by weight of absolute ethyl alcohol, heating to 70 ℃, dripping 28 parts by weight of titanium dioxide sol at a dripping speed of 1 drop/s, reacting for 12 hours, drying in a drying oven at 65 ℃, grinding, and sieving with a 200-mesh sieve to obtain the modified titanium dioxide.
Step3, weighing 62 parts by weight of self-made ASA resin powder and 5 parts by weight of modified titanium dioxide, pouring the self-made ASA resin powder and the modified titanium dioxide into a high-speed mixer for blending, heating and extruding the mixture into a film by a double-screw extruder after blending, and cooling the film by a cooling roller to obtain an ASA film;
step4, preparing an organosilicon coating component by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials;
the preparation method of the organosilicon coating component in Step4 comprises the following steps:
step one, weighing 29 parts by weight of tetraethoxysilane, 15 parts by weight of phenyl trimethoxysilane, 4 parts by weight of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and 3 parts by weight of dimethyl dimethoxy silane, uniformly mixing and stirring to obtain a first component, weighing 23 parts by weight of isopropanol, 22 parts by weight of deionized water and 0.4 part of glacial acetic acid, uniformly mixing and stirring to obtain a second component, wherein the uniformly mixing and stirring speed is 200r/min, and the uniformly mixing and stirring time is 9min;
and step two, dropwise adding the first component into the second component under the condition of stirring, heating the second component to 60 ℃ in a water bath after the dropwise adding, and preserving heat for 8 hours to obtain the organosilicon coating component, wherein the dropwise adding speed is 2 drops/s.
Step5, rolling the organosilicon coating component on the surface of the ASA film, placing the ASA film in a baking oven at 50 ℃ for 6min, and then placing the ASA film in a baking oven at 70 ℃ for 28min to obtain the window protection film for decoration protection.
A window protection film for decoration protection comprises the following components: butyl acrylate, styrene, acrylonitrile, sodium lauryl sulfate, potassium persulfate, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, tetrabutyl titanate, ethyl orthosilicate, phenyl trimethoxysilane and dimethyl dimethoxy silane.
Comparative example 1
The window protection film for decoration protection and the preparation method thereof are approximately the same as those of the embodiment 1, and the main difference is that: comparative example 1 the ASA film in example 1 was replaced with a PET film.
Comparative example 2
The window protection film for decoration protection and the preparation method thereof are approximately the same as those of the embodiment 1, and the main difference is that: this comparative example 2 replaces the modified titanium dioxide in example 1 with unmodified titanium dioxide.
Comparative example 3
The window protection film for decoration protection and the preparation method thereof are approximately the same as those of the embodiment 1, and the main difference is that: this comparative example 3 replaces the silicone coating composition of example 1 with deionized water.
Performance testing
The window protection films for finishing prepared in examples 1 to 3 and comparative examples 1 to 3 were labeled as example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3, respectively, and then the properties of examples 1 to 3 and comparative examples 1 to 3 were examined, and specific examination methods and examination items were as follows:
1. the impact properties of examples 1-3 and comparative examples 1-3 were tested with reference to the GB/T1043-1993 standard, and the resulting impact strength data are recorded in Table 1;
2. the tensile properties of examples 1-3 and comparative examples 1-3 were tested with reference to the GB/T1040-1992 standard, and the resulting tensile strength and elongation at break data are recorded in Table 1;
3. the abrasion resistance grade was judged according to the number of scratches after the abrasion, the number of scratches was excellent between 0 and 5, the number of scratches was good between 6 and 10, the number of scratches was among 11 to 15, the number of scratches was poor between 16 and 20, and the abrasion resistance grade was recorded in table 2, by putting examples 1 to 3 and comparative examples 1 to 3 under 500g load of 000# steel wool to rub back and forth 40 times;
4. flexural strength of examples 1-3 and comparative examples 1-3 were tested with reference to ISO178 standards and the resulting flexural strength data are reported in Table 2;
5. the ultraviolet aging resistance of examples 1 to 3 and comparative examples 1 to 3 was measured by irradiating them under ultraviolet irradiation for 12 hours, and the change in the surface color after ultraviolet irradiation was recorded in Table 2;
TABLE 1 Table 1 records the impact strength, tensile strength and elongation at break data
Table 2 table of wear rating, flexural Strength and uv aging resistance data recording
As is clear from the data in table 1, the mechanical properties of the window protection films for decoration and protection in the present examples 1 to 3 are better than those of the comparative examples 1 to 3, which indicates that the ASA films prepared in the present examples 1 to 3 have better mechanical properties than the PET films, and the silicone coating component coated on the ASA films can play a role in improving the mechanical properties of the films; as shown in table 2, the abrasion resistance of the window protection film for decoration in this example 1-3 is obviously better than that of comparative example 3, which indicates that the silicone coating composition coated in this example 1-3 can improve the abrasion resistance of the film, and secondly, the window protection film for decoration in this example 1-3 has better ultraviolet resistance than that of comparative example 1-3, and in summary, the window protection film for decoration and the preparation method thereof provided in the invention have better market application prospect and can be better applied in the decoration protection industry.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The preparation method of the window protection film for decoration protection is characterized by comprising the following steps:
step1, preparing self-made ASA resin powder by using butyl acrylate, styrene and acrylonitrile as raw materials through a seed emulsion polymerization method;
step2, carrying out surface modification on nano titanium dioxide by gamma- (2, 3-glycidoxy) propyl trimethoxy silane to obtain modified titanium dioxide;
step3, weighing 58-65 parts by weight of self-made ASA resin powder and 4-5 parts by weight of modified titanium dioxide, pouring the self-made ASA resin powder and the modified titanium dioxide into a high-speed mixer for blending, heating and extruding the mixture into a film by a double-screw extruder after blending, and cooling the film by a cooling roller to obtain an ASA film;
step4, preparing an organosilicon coating component by taking tetraethoxysilane, phenyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane and dimethyl dimethoxy silane as raw materials;
step5, rolling the organosilicon coating component on the surface of the ASA film, placing the ASA film in a baking oven at 50 ℃ for 5-6min, and then placing the ASA film in a baking oven at 70 ℃ for 25-30min to obtain the window protection film for decoration and protection.
2. The method for preparing a window protection film for decoration according to claim 1, wherein the Step1 of preparing the self-made ASA resin powder comprises the steps of:
1, weighing 1-2 parts by weight of sodium dodecyl sulfate and 2-3 parts by weight of potassium persulfate, pouring the sodium dodecyl sulfate and the potassium persulfate into a flask filled with 200 parts by weight of deionized water, stirring until the sodium dodecyl sulfate and the potassium persulfate are dissolved, adding 33-35 parts by weight of butyl acrylate and 2-3 parts by weight of allyl methacrylate, introducing nitrogen for protection, heating to 70 ℃, and reacting for 3 hours at constant temperature under stirring conditions, wherein the obtained mixture is marked as a seed system;
step2, weighing 95-100 parts by weight of seed system, adding 1-2 parts by weight of cumene hydroperoxide, uniformly mixing to obtain a first system, weighing 100 parts by weight of seed system, adding 38-45 parts by weight of deionized water, 0.3-0.4 part by weight of sodium dodecyl sulfate and 0.2-0.3 part by weight of potassium persulfate, uniformly mixing again, adding 2-3 parts by weight of sodium formaldehyde sulfoxylate aqueous solution, heating to 70 ℃, and dropwise adding the first system to obtain a mixed system;
step3, weighing 45-46 parts by weight of styrene, 15-16 parts by weight of acrylonitrile, 1-2 parts by weight of cumene hydroperoxide and 0.1-0.2 part by weight of sodium dodecyl sulfate, mixing uniformly, marking the mixture as a monomer component, dripping the monomer component into a mixed system heated to 70 ℃, and performing heat preservation reaction for 35-40min to obtain an ASA mixed system;
and 4, adding 5-6% of magnesium sulfate aqueous solution into the ASA mixed system, stirring for 15-20min, performing suction filtration, washing with deionized water, and drying to obtain the self-made ASA resin powder.
3. The method for producing a window protective film for decorative protection according to claim 2, wherein the stirring speed of stirring until dissolution in the step1 is 100-200r/min, the stirring time of stirring until dissolution is 8-10min, and the stirring speed of stirring conditions in the step1 is 200r/min.
4. The method for preparing a window protection film for decoration according to claim 2, wherein the stirring speed of the uniform mixing in the step2 is 200-300r/min, the stirring time of the uniform mixing is 8-10min, the stirring speed of the uniform mixing again in the step2 is 100-200r/min, the stirring time of the uniform mixing again is 12-15min, the concentration of the sodium formaldehyde sulfoxylate aqueous solution in the step2 is 0.25mg/L, and the dripping speed in the step2 is 1-2 drops/s.
5. The method for preparing a window protection film for decoration according to claim 2, wherein the stirring speed of the fully and uniformly mixing in the step3 is 100-200r/min, the stirring time of the fully and uniformly mixing is 12-15min, and the dripping speed in the step3 is 1-2 drops/s.
6. The method for preparing a window protection film for decoration according to claim 2, wherein the mass concentration of the magnesium sulfate aqueous solution in the step4 is 10%, the stirring speed in the step4 is 100-200r/min, the drying temperature in the step4 is 70 ℃, and the drying time is 24h.
7. The method for producing a window protective film for decorative protection according to claim 1, wherein the Step of producing the modified titania in Step2 comprises:
step A, absolute ethyl alcohol and glacial acetic acid are mixed according to a ratio of 3:1, stirring for 3-5min at a stirring speed of 300-500r/min, dripping tetrabutyl titanate with 5-8% of the weight of the tetrabutyl titanate, and stirring for 30min at a stirring speed of 800-1000r/min under a water bath condition at 30 ℃ to obtain a component to be reacted;
step B, adjusting the pH value of a component to be reacted to 1 by using hydrochloric acid with the concentration of 1mol/L, then dripping ethanol aqueous solution with the mass concentration of 60% and the weight of 35-40% into the component at the dripping speed of 1 drop/s, heating the solution to 70 ℃ and then reacting for 12 hours to obtain the titanium dioxide sol;
and C, weighing 8-10 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, dispersing into 100 parts by weight of absolute ethyl alcohol, heating to 70 ℃, dripping 25-30 parts by weight of titanium dioxide sol at a dripping speed of 1 drop/s, reacting for 12 hours, drying in a drying oven at 65 ℃, grinding, and sieving with a 200-mesh sieve to obtain the modified titanium dioxide.
8. The method for preparing a window protection film for decoration according to claim 1, wherein the Step4 of preparing the silicone coating component comprises the steps of:
step one, weighing 28-30 parts by weight of tetraethoxysilane, 14-15 parts by weight of phenyl trimethoxysilane, 3-4 parts by weight of gamma- (2, 3-glycidoxy) propyl trimethoxysilane and 2-3 parts by weight of dimethyl dimethoxy silane, mixing and stirring uniformly to obtain a first component, weighing 22-25 parts by weight of isopropanol, 22-23 parts by weight of deionized water and 0.3-0.4 part of glacial acetic acid, mixing and stirring uniformly to obtain a second component;
and step two, dropwise adding the first component into the second component under the condition of stirring, heating the second component to 60 ℃ in a water bath after the dropwise adding, and preserving the heat for 8 hours to obtain the organosilicon coating component.
9. The method for preparing a window protection film for decoration according to claim 8, wherein the stirring speed of the uniform mixing and stirring in the first step is 100-200r/min, the stirring time of the uniform mixing and stirring is 8-10min, and the dripping speed in the second step is 1-2 drops/s.
10. A window protection film for decoration protection, characterized by being produced by a process for producing a window protection film for decoration protection according to any one of claims 1 to 9, the components of the window protection film for decoration protection comprising: butyl acrylate, styrene, acrylonitrile, sodium lauryl sulfate, potassium persulfate, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, tetrabutyl titanate, ethyl orthosilicate, phenyl trimethoxysilane and dimethyl dimethoxy silane.
CN202410102324.XA 2024-01-25 2024-01-25 Window protection film for decoration protection and preparation method thereof Pending CN117624695A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202410102324.XA CN117624695A (en) 2024-01-25 2024-01-25 Window protection film for decoration protection and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202410102324.XA CN117624695A (en) 2024-01-25 2024-01-25 Window protection film for decoration protection and preparation method thereof

Publications (1)

Publication Number Publication Date
CN117624695A true CN117624695A (en) 2024-03-01

Family

ID=90021936

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202410102324.XA Pending CN117624695A (en) 2024-01-25 2024-01-25 Window protection film for decoration protection and preparation method thereof

Country Status (1)

Country Link
CN (1) CN117624695A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102167876A (en) * 2011-01-17 2011-08-31 合肥工业大学 Butyl acrylate-styrene-acrylonitrile copolymer/titanium dioxide composite film and preparation method thereof
CN116102831A (en) * 2023-04-12 2023-05-12 广州市雄星塑料制品有限公司 Explosion-proof cold-proof UV-resistant PVC film and preparation process thereof
CN116285431A (en) * 2023-03-16 2023-06-23 安徽五星高新材料有限公司 Preparation method of aluminum pigment with high affinity with resin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102167876A (en) * 2011-01-17 2011-08-31 合肥工业大学 Butyl acrylate-styrene-acrylonitrile copolymer/titanium dioxide composite film and preparation method thereof
CN116285431A (en) * 2023-03-16 2023-06-23 安徽五星高新材料有限公司 Preparation method of aluminum pigment with high affinity with resin
CN116102831A (en) * 2023-04-12 2023-05-12 广州市雄星塑料制品有限公司 Explosion-proof cold-proof UV-resistant PVC film and preparation process thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈良兵等: "聚酯薄膜用高韧性无底涂耐磨硅树脂的制备", 化工新型材料, vol. 46, no. 4, 30 April 2018 (2018-04-30), pages 104 - 107 *

Similar Documents

Publication Publication Date Title
CN101348595B (en) Fluorine-silicon modified self-crosslinking acrylic ester emulsion preparation method
CN105176371A (en) Ultraviolet curing coating and preparation method thereof, and super-hydrophilic transparent antifogging coating layer and preparation method thereof
CN105176293B (en) Super hydrophilic coating and preparation method thereof and super-hydrophilic coating and preparation method
CN107880754A (en) A kind of compound heat-insulating energy-saving paint of polyurethane-modified polyacrylate and preparation method thereof
CN111073433B (en) Exterior wall heat-insulating coating and preparation method thereof
KR100918623B1 (en) Antibiotic and waterproof composition for coating natural ventilating device, natural ventilating device prepared therefrom and preparation method thereof
JPS6033858B2 (en) Coating composition
JPS6375074A (en) Coating composition
CN113278322A (en) Stone-like paint and preparation method thereof
CN117624695A (en) Window protection film for decoration protection and preparation method thereof
CN110437776A (en) A kind of double-component aqueous redwood splicing adhesive and its application
CN111875756A (en) Preparation method and formula of soap-free synthetic aqueous acrylic acid dispersion resin
CN112266169A (en) Stone-like glass mosaic and preparation method thereof
CN1238449C (en) Organic montmorrilonite modified silicon polyacrylicresin outer wall paint
CN112280376B (en) High-sun-proof printing ink for impregnated paper and preparation method thereof
CN116285661A (en) Anti-reflection film capable of being cured at normal temperature and preparation method thereof
CN106634370A (en) Environment-friendly scrubbing-resistant automobile heat-preservation color-retention heat-insulation paint and preparation method thereof
JPH079482B2 (en) Method for producing synthetic resin lens having dye-cured surface layer
CN109929361A (en) Dead color system reflective heat-insulation paint and preparation method thereof
CN111073365A (en) Fluorocarbon coating for aluminum curtain wall board and spraying process thereof
CN115044281B (en) Preparation method and application of ultraviolet light curing finishing paint prepared from modified ball clay
CN114539837B (en) Sun-proof paint for dyed wood and coating method thereof
CN115991958B (en) Novel fluorine-containing weather-resistant coating and preparation and use methods thereof
CN115895438B (en) Transparent organic silicon coating for polycarbonate surface and preparation method thereof
CN114685926B (en) ASA coated PVC wood-plastic co-extrusion section bar

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination