CN113736267A - Reversibly-stretched shading organic silicon film and preparation method thereof - Google Patents
Reversibly-stretched shading organic silicon film and preparation method thereof Download PDFInfo
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- CN113736267A CN113736267A CN202111134700.6A CN202111134700A CN113736267A CN 113736267 A CN113736267 A CN 113736267A CN 202111134700 A CN202111134700 A CN 202111134700A CN 113736267 A CN113736267 A CN 113736267A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 54
- 239000010703 silicon Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 124
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 121
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229920001971 elastomer Polymers 0.000 claims abstract description 46
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 43
- 229920002050 silicone resin Polymers 0.000 claims abstract description 43
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 239000003112 inhibitor Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- 229910004674 SiO0.5 Inorganic materials 0.000 claims description 28
- 229910052681 coesite Inorganic materials 0.000 claims description 24
- 229910052906 cristobalite Inorganic materials 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 24
- 229910052682 stishovite Inorganic materials 0.000 claims description 24
- 229910052905 tridymite Inorganic materials 0.000 claims description 24
- 229920006268 silicone film Polymers 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- -1 olefin siloxane Chemical class 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910020381 SiO1.5 Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910014307 bSiO Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 125000003118 aryl group Chemical group 0.000 claims 2
- 239000003208 petroleum Substances 0.000 claims 1
- 230000002087 whitening effect Effects 0.000 abstract description 9
- 230000005540 biological transmission Effects 0.000 abstract description 8
- 230000002441 reversible effect Effects 0.000 abstract description 6
- 238000007259 addition reaction Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 71
- 238000002834 transmittance Methods 0.000 description 18
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 12
- 239000011737 fluorine Substances 0.000 description 12
- 229910052731 fluorine Inorganic materials 0.000 description 12
- 238000001816 cooling Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000004945 silicone rubber Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000003849 aromatic solvent Substances 0.000 description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000003759 ester based solvent Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
Abstract
The invention discloses a reversibly-stretched shading organic silicon film and a preparation method thereof, wherein the reversibly-stretched shading organic silicon film comprises the following components in parts by weight: 100 parts of vinyl silicone crude rubber, 150-500 parts of vinyl silicone resin, 1-4 parts of a cross-linking agent, 0.05-0.5 part of an inhibitor, 0.5-2 parts of a platinum catalyst and 20-100 parts of a solvent. The invention mixes the vinyl silicone crude rubber and vinyl silicone resin with a cross-linking agent, an inhibitor, a platinum catalyst and a solvent, coats the mixture to form a film, heats and cures the film, so that the vinyl silicone crude rubber and the vinyl silicone resin are subjected to addition reaction under the action of the platinum catalyst to form a film with certain cohesive strength, the film has good light transmission performance in an initial state, obvious whitening and shading phenomena occur after stretching, the film is recovered to the initial light transmission state after the stretching force is removed, the reversible stretching and shading functions of the organic silicon film are realized, and the invention has certain potential application scenes, such as bus window shading and the like.
Description
Technical Field
The invention relates to the technical field of organic silicon films, in particular to a reversibly-stretched shading organic silicon film and a preparation method thereof.
Background
The phenomenon that a stretching area is whitish often occurs when a high polymer plastic film such as PP, PE and the like is stretched and bent by external force, so that the light transmittance of the plastic film is changed. Bucknell and Smith reports (Polymer,1965,6,437) the relationship between whitening and the silver streaks of polymeric materials, and they found that in the stress-whitened region, the Polymer density decreased, the refractive index decreased, and the occurrence of whitening was caused. In order to recover the stress whitening phenomenon of the polymer thin film, it is necessary to heat-treat them.
The organic silicon high molecular material comprises organic silicon oil, organic silicon crude rubber and organic silicon resin, and products taking the organic silicon high molecular material as raw materials, such as organic silicon pressure-sensitive adhesive, organic silicon sealant, organic silicon heat-conducting adhesive, organic silicon rubber products and the like, are widely applied to various industries. The base material has a flexible one-dimensional chain structure, so that an obvious stretching phenomenon can occur under the action of external force, and the original state can be recovered after the external force is removed, so that most of organosilicon materials can show better elasticity.
When the organic silicon film is stretched by external force, the sea-island structure in the molecular structure of the organic silicon film is stretched and adjusted, the distribution of resin in the structure is changed, the regional density and the refractive index are changed, and the stretching and whitening phenomenon is caused. If the whitening phenomenon occurs, the light transmission performance of the organic silicon film is obviously changed, the light transmission organic silicon film is gradually transited to the shading organic silicon film, and the organic silicon film can be quickly and reversibly restored to the light transmission state by utilizing the elasticity, namely small permanent deformation, of the organic silicon film. The prior organic silicon film still keeps high light transmittance performance during stretching, and the phenomenon of stretching whitening does not occur.
In patent CN110646870A, an organosilicon film with adjustable light transmittance and a preparation method thereof are disclosed, wherein a transparent elastic film is pre-stretched, a hard layer is formed by surface treatment, and then secondary stretching is performed to obtain an organosilicon film with adjustable light transmittance; in patent CN108424543B, an organosilicon film preparation method for regulating and controlling light transmittance through surface wrinkles is disclosed, in which a transparent elastic substrate is subjected to plasma etching to form a hydrophilic layer, and then a layer of rigid composite film solution is coated and dried to form a film, and a light transmittance adjustable film is formed by stretching to release stress. The process required for preparing the organic silicon film with adjustable light transmittance is complicated, the prepared organic silicon film with adjustable light transmittance needs the matching of a double-layer structure, the elastic layer is combined with the hard layer or the rigid structure, and finally the hard layer and the rigid structure play a light transmittance adjusting function. Therefore, we propose a reversible stretch light-shielding silicone film and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a reversible stretching shading organic silicon film and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a reversible stretch shading organic silicon film comprises the following components in parts by weight: 100 parts of vinyl silicone crude rubber, 150-500 parts of vinyl silicone resin, 1-4 parts of a cross-linking agent, 0.05-0.5 part of an inhibitor, 0.5-2 parts of a platinum catalyst and 20-100 parts of a solvent.
Further, the mass ratio of the vinyl silicone raw rubber to the vinyl silicone resin is 0.10 to 0.80, and more preferably 0.20 to 0.67.
Furthermore, the molar ratio of silicon hydrogen to vinyl in the raw material composition is 0.3-10, and more preferably 0.5-5.
Further, the vinyl silicone crude rubber has a general formula:
ViaR1 3-aSi(VibR1 2-bSiO)n(R1 2SiO)mSiR1 3-aVia；
wherein R is1Saturated alkyl or aromatic alkyl with 1-10 carbon atoms, such as methyl, ethyl, propyl, butyl, cyclohexyl, etc., and aromatic alkyl such as phenyl, benzyl, phenethyl, etc.; m and n are integers, and the molecular weight of the vinyl silicon crude rubber is more than 40 ten thousand; a is an integer of 0-3; b is an integer of 0 to 2.
Specific examples of vinyl silicone gums can be, but are not limited to:
ViMe2Si(ViMeSiO)n(Me2SiO)mSiMe2Vi；
Vi2MeSi(ViMeSiO)n(Me2SiO)mSiMeVi2；
ViPh2Si(ViPhSiO)n(Ph2SiO)mSiPh2Vi；
Vi2PhSi(ViPhSiO)n(Ph2SiO)mSiPhVi2；
ViMe2Si(ViMeSiO)n(Me2SiO)0.9m(Ph2SiO)0.1mSiMe2Vi；
Vi2MeSi(ViMeSiO)n(Me2SiO)0.9m(Ph2SiO)0.1mSiMeVi2；
ViMe2Si(Me2SiO)mSiMe2Vi；
Vi2MeSi(Me2SiO)mSiMeVi2；
ViPh2Si(Ph2SiO)mSiPh2Vi；
Vi2PhSi(Ph2SiO)mSiPhVi2；
ViMe2Si(Me2SiO)0.9m(Ph2SiO)0.1mSiMe2Vi；
Vi2MeSi(Me2SiO)0.9m(Ph2SiO)0.1mSiMeVi2and the like.
Further, the number of non-methyl groups in the vinyl silicone gum is not more than 10% of all substituents, more preferably not more than 3%.
Furthermore, the vinyl silicon raw rubber has a vinyl group mole percentage of 0.01-0.50%, and more preferably 0.01-0.20%.
Further, the vinyl silicone resin has a general formula:
(VicR2 3-cSiO0.5)h(VidR2 2-dSiO)i(VieR2 1-eSiO1.5)j(SiO2)k；
wherein R is2Saturated alkyl or aromatic alkyl with 1-10 carbon atoms, such as methyl, ethyl, propyl, butyl, cyclohexyl, etc., and aromatic alkyl such as phenyl, benzyl, phenethyl, etc.; c is an integer of 1 to 3, d is an integer of 0 to 2, and e is 0 to 1An integer number;
the ratio of h/(i + j + k) is 0.2-1.2, preferably 0.5-1.0, and more preferably 0.7-0.9;
the molecular weight of the vinyl silicone resin is 1000-10000, preferably 2000-8000, more preferably 3000-5000;
specific examples of vinyl silicone resins may be, but are not limited to:
(ViMe2SiO0.5)h(SiO2)k；
(Vi2MeSiO0.5)h(SiO2)k；
(ViPh2SiO0.5)h(SiO2)k；
(Vi2PhSiO0.5)h(SiO2)k；
(ViMe2SiO0.5)h(MeSiO1.5)j(SiO2)k；
(Vi2MeSiO0.5)h(MeSiO1.5)j(SiO2)k；
(ViPh2SiO0.5)h(MeSiO1.5)j(SiO2)k；
(Vi2PhSiO0.5)h(MeSiO1.5)j(SiO2)k；
(ViMe2SiO0.5)h(Me2SiO)i(MeSiO1.5)j(SiO2)k；
(Vi2MeSiO0.5)h(Me2SiO)i(MeSiO1.5)j(SiO2)k；
(ViPh2SiO0.5)h(Me2SiO)i(MeSiO1.5)j(SiO2)k；
(Vi2PhSiO0.5)h(Me2SiO)i(MeSiO1.5)j(SiO2)kand the like.
Further, the mol percentage of vinyl in the vinyl silicone resin is 0.02% to 2.0%, and more preferably 0.05% to 1.6%.
Further, the crosslinking agent has a viscosity of 1 to 50 mPas at 25 ℃.
Further, the weight percentage of hydrogen in the cross-linking agent is 0.01-3%; more preferably 0.01% to 1.8%.
Further, the inhibitor can be selected from alkynol organic matters with the boiling point of 50-200 ℃.
Further, the platinum catalyst may be selected from, but not limited to, platinum black, chloroplatinic acid, platinum/olefin siloxane coordination compounds.
Furthermore, the solvent can be selected from aliphatic solvents, aromatic solvents and ester solvents; fats such as hexane, heptane, cyclohexane, mineral spirits; aromatic solvents such as toluene, xylene, etc.; ester solvents such as ethyl acetate, methyl acetate; the solvent is one or more of the above components.
A preparation method of a reversibly stretchable shading organic silicon film comprises the following preparation processes:
mixing vinyl silicone resin and a solvent, stirring until the vinyl silicone resin is fully dissolved, adding vinyl silicone crude rubber, a cross-linking agent and an inhibitor, stirring at room temperature until the vinyl silicone crude rubber, the cross-linking agent and the inhibitor are fully dissolved and mixed, and in order to shorten the time, heating to about 80 ℃, fully stirring and dissolving, and then cooling to the room temperature; adding a platinum catalyst, uniformly mixing, coating on a fluorine release film, drying at 60 ℃ for 15-60 min, and removing the solvent; curing at 110-150 ℃ for 3-15 min, rolling, and removing the release film in the using process to obtain the organic silicon film.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention relates to a reversibly-stretched shading organic silicon film and a preparation method thereof, which are characterized in that vinyl silicone raw rubber and vinyl silicone resin are mixed with a cross-linking agent, an inhibitor, a platinum catalyst and a solvent, coated to form a film, and heated and cured, so that the vinyl silicone raw rubber and the vinyl silicone resin are subjected to hydrosilylation under the action of the platinum catalyst to form the film with certain cohesive strength, the film has good light transmittance in an initial state, and is subjected to obvious whitening shading phenomenon after being stretched, and is recovered to the initial light transmittance state after the tension is removed, so that the reversibly-stretched shading function of the organic silicon film is realized, and the reversibly-stretched shading organic silicon film has a certain potential application scene, such as shading of bus windows and the like.
2. The invention discloses a reversible stretching shading organic silicon film and a preparation method thereof, discloses the dosage of vinyl silicone resin, and has a key influence on the stretching whitening phenomenon; the increase of the usage amount of the vinyl silicone resin enables redistribution in a cross-linking structure in the stretching process to be more obvious, the stretching shading effect of the prepared organic silicon film is obviously improved, but the excessive vinyl silicone resin enables the organic silicon film to show plasticity while showing elasticity, generate permanent deformation after stretching, and need to be subjected to heat treatment to recover the initial light transmission performance; and the preparation process of the organic silicon film is simple, and the light transmission adjusting function of the organic silicon film can be realized only by a single-layer structure.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 200 parts by mass of vinyl silicone resin B1 and 40 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 2
Adding 300 parts by mass of vinyl silicone resin B1 and 60 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 3
Adding 400 parts by mass of vinyl silicone resin B1 and 80 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 4
Adding 500 parts by mass of vinyl silicone resin B1 and 100 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 5
Adding 300 parts by mass of vinyl silicone resin B2 and 40 parts by mass of solvent toluene into a 2L planetary stirrer, after B2 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B2: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.12%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 6
Adding 300 parts by mass of vinyl silicone resin B2 and 40 parts by mass of solvent toluene into a 2L planetary stirrer, after B2 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A2, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A2: the raw silicone rubber only contains terminal vinyl, the vinyl mole fraction is 0.03 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B2: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.12%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Example 7
Adding 300 parts by mass of vinyl silicone resin B1 and 40 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A2, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A2: the raw silicone rubber only contains terminal vinyl, the vinyl mole fraction is 0.03 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Comparative example 1
Adding 80 parts by mass of vinyl silicone resin B1 and 20 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Comparative example 2
Adding 80 parts by mass of vinyl silicone resin B2 and 20 parts by mass of solvent toluene into a 2L planetary stirrer, after B2 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A1, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A1: the silicone crude rubber contains terminal vinyl and side chain vinyl, the vinyl mole fraction is 0.10 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B2: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.12%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Comparative example 3
Adding 80 parts by mass of vinyl silicone resin B1 and 20 parts by mass of solvent toluene into a 2L planetary stirrer, after B1 is fully dissolved, adding 100 parts by mass of vinyl silicone crude rubber A2, 2 parts by mass of cross-linking agent and 0.1 part by mass of inhibitor cyclohexylynol, stirring at 80 ℃ until fully dissolved and mixed, and cooling to room temperature; adding 0.5 parts by mass of platinum catalyst (CA 28, platinum content 2000ppm) and mixing, coating on fluorine release film, drying at 60 deg.C for 30min, and removing solvent; curing at 150 ℃ for 6min, and stripping the release film to obtain the organic silicon film.
Wherein the vinyl silicone crude rubber A2: the raw silicone rubber only contains terminal vinyl, the vinyl mole fraction is 0.03 percent, and the molecular weight is 60 ten thousand;
vinyl silicone resin B1: from ViMe2SiO0.5Unit, Me3SiO0.5Unit and SiO2The unit composition, the mass fraction of vinyl is 0.08%;
the crosslinking agent had a hydrogen content of 0.80% and a viscosity of 10 mPas.
Experiment of
The silicone films obtained in examples 1 to 7 and comparative examples 1 to 3 were used to prepare samples, and the properties thereof were measured and the measurement results were recorded:
and (3) testing tensile strength: coating the organic silicon film on the fluorine release film to a thickness of 1.5mm to obtain a sample, cutting the sample into strips of 2cm multiplied by 4cm, and testing by using a tensile machine;
and (3) testing light transmittance: detecting the light transmittance of the sample at 550nm by using a handheld light transmittance tester;
the experiments were all carried out at 25 ℃.
From the data in the table above, it is clear that the following conclusions can be drawn:
the silicone films obtained in examples 1 to 7 were compared with the silicone films obtained in comparative examples 1 to 3, and the results of the measurements were found to be,
1. the silicone films obtained in examples 1 to 4 were compared with each other, and it is understood from the data in the table that the stretching and light-shielding effects of the silicone films become more remarkable as the amount of the vinyl silicon resin added increases;
because the vinyl silicone resin is too much, the organic silicon film obtained in the example 4 not only shows certain elasticity, but also shows certain plasticity, has permanent deformation after being stretched, and needs to be treated at the temperature of more than 70 ℃ for about 10min in order to recover the initial light transmittance;
2. as can be seen from the data in the tables, the elastic silicone films obtained in examples 5 to 7 have an obvious stretching and light-shielding effect, and the light transmittance of the films is restored to the initial state after the external force is removed;
3. the data in the tables show that the silicone films obtained in comparative examples 1 to 3 still maintain relatively good light transmission performance after being stretched;
4. the silicone films obtained in examples 1 to 7 had lower light transmittance after stretching by 30% compared to the silicone films obtained in comparative examples 1 to 3, and the light transmittance of the samples was restored to a good level after the tensile force was removed, which fully indicates that the present invention achieves the reversible stretch-blocking function of the silicone films produced.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A reversibly stretchable light-shielding organic silicon film is characterized in that: comprises the following components by weight: 100 parts of vinyl silicone crude rubber, 150-500 parts of vinyl silicone resin, 1-4 parts of a cross-linking agent, 0.05-0.5 part of an inhibitor, 0.5-2 parts of a platinum catalyst and 20-100 parts of a solvent.
2. The reversibly stretchable light-screening silicone film according to claim 1, characterized in that: the mass ratio of the vinyl silicone crude rubber to the vinyl silicone resin is 0.20-0.67.
3. The reversibly stretchable light-screening silicone film according to claim 1, characterized in that: the molar ratio of silicon hydrogen to vinyl in the raw material composition is 0.5-5.
4. A reversibly stretchable light-screening silicone film according to any one of claims 1 to 3, characterized in that: the vinyl silicon crude rubber has a general formula as follows: viaR1 3-aSi(VibR1 2-bSiO)n(R1 2SiO)mSiR1 3-aVia；
Wherein R1 is a saturated alkyl or aromatic alkyl group having 1 to 10 carbon atoms, Vi is a vinyl group, a is an integer of 0 to 3, and b is an integer of 0 to 2.
5. The reversibly stretchable light-screening silicone film according to claim 4, characterized in that: the molecular weight of the vinyl silicon crude rubber is 40-80 ten thousand, and the mol percentage of vinyl is 0.01-0.20%.
6. A reversibly stretchable light-screening silicone film according to any one of claims 1 to 3, characterized in that: the vinyl silicone resin has a general formula: (Vi)cR2 3-cSiO0.5)h(VidR2 2-dSiO)i(VieR2 1-eSiO1.5)j(SiO2)k；
Wherein R is2Is a saturated alkyl or aromatic alkyl group having 1 to 10 carbon atoms, Vi is a vinyl group, c is an integer of 1 to 3, d is an integer of 0 to 2, and e is an integer of 0 to 1; the ratio of h/(i + j + k) is 0.2-1.2.
7. The reversibly stretchable light-screening silicone film according to claim 6, characterized in that: the molecular weight of the vinyl silicone resin is 1000-10000, and the mol percentage of vinyl is 0.05-1.6%.
8. The reversibly stretchable light-screening silicone film according to claim 1, characterized in that: the viscosity of the cross-linking agent at 25 ℃ is 1-50 mPa.s, and the mass percentage of hydrogen is 0.01-1.8%.
9. The reversibly stretchable light-screening silicone film according to claim 1, characterized in that: the platinum catalyst is one of platinum black, chloroplatinic acid and platinum/olefin siloxane coordination compounds;
the solvent is one or a mixture of toluene, xylene, petroleum ether, solvent oil and ethyl acetate.
10. A preparation method of a reversibly stretchable shading organic silicon film is characterized by comprising the following steps: the preparation method comprises the following preparation processes:
mixing vinyl silicone resin and a solvent, stirring until the vinyl silicone resin is fully dissolved, adding vinyl silicone crude rubber, a cross-linking agent and an inhibitor, and stirring until the vinyl silicone crude rubber, the cross-linking agent and the inhibitor are fully dissolved and mixed; adding a platinum catalyst, uniformly mixing, coating, drying at 60 ℃ for 15-60 min, and curing at 110-150 ℃ for 3-15 min to obtain the organic silicon film.
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