CN117624695A - Window protection film for decoration protection and preparation method thereof - Google Patents
Window protection film for decoration protection and preparation method thereof Download PDFInfo
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- 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
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- 238000005034 decoration Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000004224 protection Effects 0.000 title claims description 78
- 238000002156 mixing Methods 0.000 claims abstract description 74
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 24
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 17
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 17
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 238000010556 emulsion polymerization method Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 130
- 238000005303 weighing Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 30
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000007864 aqueous solution Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 25
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 24
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 20
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 17
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 15
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 10
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000004447 silicone coating Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000006750 UV protection Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 19
- 238000005299 abrasion Methods 0.000 description 6
- 239000002985 plastic film Substances 0.000 description 5
- 229920006255 plastic film Polymers 0.000 description 5
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical class O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007730 finishing process Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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
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.
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