CN103627334B - Photochromic film, photochromic glass and preparation method - Google Patents
Photochromic film, photochromic glass and preparation method Download PDFInfo
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- CN103627334B CN103627334B CN201210306996.XA CN201210306996A CN103627334B CN 103627334 B CN103627334 B CN 103627334B CN 201210306996 A CN201210306996 A CN 201210306996A CN 103627334 B CN103627334 B CN 103627334B
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Abstract
The present invention is applicable to glass technology field, provides a kind of organic photochromic film, organic photochromic glass and preparation method.Photochromic glass of the present invention comprises the first mutually stacked glass coating, the second glass coating, the first PVB layer, the second PVB layer and photochromic film, this first PVB layer, the second PVB layer are stacked to be incorporated between this first glass coating and second glass coating, and this photochromic film is stacked to be incorporated between the first PVB layer, the second PVB layer.Photochromic glass of the present invention, realizes discoloration by said structure and greatly improves.
Description
Technical field
The invention belongs to glass technology field, particularly relate to a kind of photochromic film, photochromic glass and preparation method.
Background technology
Doubling glass two panels or divided glass to be pasted with film to form, also referred to as laminated glass or glyglass under certain temperature and pressure.Film is the film such as PVB (Polyvinyl butyral, polyvinyl butyral acetal) normally.Doubling glass still keeps high permeability to the visible ray in sunlight, infrared rays, causes energy-saving effect poor.
Photochromic glass is a kind of novel energy-saving glass, and when illumination strengthens, glass tarnishes gradually, reduces light and carries the transmitance of heat; When illumination weakens, glass recovers again bright, improves light and carries the transmitance of heat.Thisly with sooner or later and the environmental change in the four seasons, and can automatically change the intelligent glass of transmittance and shading coefficient, there is the advantage not available for star's energy-saving glass such as Low emissivity Low-E, caused the special concern of people.
At present, have and photochromic for multilayer hard board clip is held between two blocks of sheet glass, obtained a kind of photochromic sandwich glass; Also have and argent and halogen simple substance are joined in other frit respectively, obtained a kind of lens blank with photochromic effect; Or adopt heat treating process or reduction treatment legal system to produce a kind of bulk glass of colour-changed due to gradual light-changing; Even some directly to install the photo chromic glass such as traditional silver halide respectively on the vehicle body of car, automobile, commercial vehicle and passenger vehicle.In addition, the patent of also some photochromic glass abroad, but be mostly the improvement opportunity to silver halide and photosensitizer system, and electrochromic substance is all in glass body.But, there is not the PVB film that organic photochromic material makes and laminated glass thereof so far.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of photochromic film, photochromic glass and preparation method thereof with good discoloration.
The present invention is achieved in that
A kind of photochromic film, is characterized in that, comprise the component of following weight percent:
The present invention also provides a kind of photochromic glass, comprise the first mutually stacked glass coating, the second glass coating, the first PVB layer, the second PVB layer and above-mentioned photochromic film, this first PVB layer, the second PVB layer are stacked to be incorporated between this first glass coating and second glass coating, and this photochromic film is stacked to be combined between this first PVB layer, the second PVB layer.
The present invention further provides above-mentioned photochromic glass preparation method, comprise the steps:
First glass coating, the second glass coating, the first PVB layer, the second PVB layer and above-mentioned photochromic film are provided;
Described first PVB layer, the second PVB layer are laminated between described first glass coating and the second glass coating, described photochromic film layers are stacked between the first PVB layer, the second PVB layer, obtain photochromic glass through hot pressing.
The photochromic film of the present invention, by using organic photochromic powder, the interphase interaction of this organic photochromic powder and softening agent, coupling agent, realizes its discoloration and greatly improves.
Photochromic glass of the present invention, by using above-mentioned photochromic film, realizes its discoloration and greatly promotes.
Photochromic glass preparation method of the present invention, with low cost, environmental pollution is little, and prepared photochromic glass has good discoloration.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention photochromic glass structure iron.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A kind of photochromic film, is characterized in that, comprise the component of following weight percent:
Particularly, organic photochromic powder contained in the photochromic film of the embodiment of the present invention is selected from spiropyran and derivative (such as 1' thereof, 3', 3'-trimethylammonium-6-hydroxyl spiral [2H-1-chromene-2,2'-indoline]), acyl is for one or more in aniline (such as 4'-chloro pivalyl aniline), schiff bases (such as 1,8-naphthalimide), osazone (such as D-Glucose osazone).If above-mentioned various organic photochromic powder forms by two kinds, there is no weight limits between the two.The weight percent of this photochromic powder is 0.01% ~ 2%, such as 1%, 0.5%, 0.35wt%, 1.5% etc.The discoloration of photochromic film can increase with the content of color-change powder and improve, but too much color-change powder can reduce the visible light transmittance rate of film, and the preferred weight percent of color-change powder in photochromic film is 0.5% ~ 2%, is preferably 1%.
This softening agent be selected from the two positive heptanoate of triglycol, triglycol two 2-ethylhexoate, dioctyl phthalate (DOP), dimixo-octyl phthalate more than one, the content of this softening agent is 0.3% ~ 2.0%, is preferably 1%.Plasticizer loading height can affect the workability, high temperature resistant of the photochromic film that polyvinyl butyral acetal generates, low temperature, mechanical property etc.
This coupling agent selects vinyltriethoxysilane, 3-methacryloxypropyl trimethoxy silane coupling agent, hexanediamine ylmethyl triethoxyl silane, more than one in Y-aminopropyl triethoxysilane, the content of this coupling agent is 0.2% ~ 1.0%, is preferably 0.8%.Coupling agent content height can affect the photochromic film of polyvinyl butyral acetal generation and the adhesive property etc. of glass.
The consumption of this polyvinyl butyral acetal (PVB) is 95% ~ 99%.Organic photochromic powder is even
Be dispersed in variable color film PVB carrier, make compact construction, do not change the basic structure of existing doubling glass, drop into lower, but there is efficient photochromic effect.
Above-mentioned each organic photochromic powder can be commercially available prod.
Preferably, as one embodiment of the invention, the thickness of this photochromic film is 0.38 ~ 3.04 millimeter, and photochromic energy-saving effect can increase along with film stock thickness and improve, but can increase materials cost simultaneously, and preferred thickness is 0.76 millimeter.
Particularly, this photochromic film preparation method, comprises the steps:
Polyvinyl alcohol contracting butyl aldehyde, softening agent, coupling agent and above-mentioned photochromic powder are provided, by described photochromic powder, polyvinyl butyral acetal, softening agent and coupling agent by following weight percent mixing, obtain mixture;
This mixture is added in mixing roll and stirs 10 ~ 20 minutes, be heated to 140 ~ 160 DEG C and melt and extrude and make the film of 0.38 ~ 3.04 millimeter, then by after cool, anhydrate, dry up etc. and operating, obtain photochromic film; The weight percent of each component is as follows:
Particularly, this polyvinyl alcohol contracting butyl aldehyde, softening agent, coupling agent and photochromic powder are identical with aforementioned, do not repeat to set forth at this.
The photochromic film of the embodiment of the present invention, by selecting above-mentioned photochromic powder, has better color changeable effect.
The embodiment of the present invention also provides a kind of photochromic glass.This photochromic glass structure as shown in Figure 1, comprise the first mutually stacked glass coating 4, second glass coating 5, first PVB layer 1, second PVB layer 2 and photochromic film 3, this the first PVB layer 1, second PVB layer 2 is laminated in conjunction with between this first glass coating 4 and the second glass coating 5, and this photochromic film 3 is stacked to be combined between this first PVB layer 1, second PVB layer 2.Wherein, the position of the first PVB layer 1, second PVB layer 2 can exchange, and like this, the present embodiment photochromic glass at least has following preferred structure:
As a preferred embodiment, the first glass coating 4, PVB first PVB layer 1, photochromic film 3, PVB second PVB layer 2, second glass coating 5 stack gradually combination, and its structure as shown in Figure 1.
Particularly, the photochromic film 3 in the various embodiments described above is all consistent on component, content and thickness with aforesaid photochromic film, does not repeat to set forth at this.
Preferably but be not only only common float glass or ultra-white float glass, thickness all can be 1.6mm ~ 3.0mm to the material of this first glass coating 1 and the second glass coating 2.
The material of this first PVB layer and the second PVB layer is PVB film, and thickness is 0.38mm ~ 1.14mm.
Embodiment of the present invention photochromic glass, by selecting above-mentioned variable color film, has better color changeable effect.
The embodiment of the present invention provides above-mentioned photochromic glass preparation method further, comprises the steps:
Step S01, provides the first glass coating, the second glass coating, the first PVB layer, the second PVB layer and described photochromic film;
Step S02, prepares photochromic glass:
To be laminated between this first glass coating and second glass coating by this first PVB layer, the second PVB layer in step S01, this photochromic film layers be stacked between this first PVB layer, the second PVB layer, hot pressing obtains photochromic glass.
Particularly, in step S01, the recipe ingredient of photochromic film, preparation method and thickness as described above, in order to save length, do not repeat them here.First glass coating, the second glass coating, the first PVB layer, the second PVB layer are identical with aforesaid, do not repeat to set forth at this
In step S02, first glass coating, the second glass coating, the first PVB layer, area equation between the second PVB layer and photochromic film, put in the lump in silica gel bag after stacked, under 2.5KPa vacuum tightness, be vented 20 minutes and transfer in drying oven 85 DEG C of insulations 30 minutes; Then, in autoclave, hot-pressing processing, the processing condition of hot-pressing processing are hot pressing temperature is 110 ~ 150 DEG C, and pressure is 1.0 ~ 3MPa, and at preferred 1.3MPa pressure and 135 DEG C, hot pressing 25 minutes, obtains photochromic glass.If temperature and pressure is not enough during hot pressing, be difficult to form doubling glass; On the contrary, if temperature is too high, meeting decomposing oxalic acid and polyvinyl butyral acetal, destroy the structure of photochromic films.
Embodiment of the present invention photochromic glass irradiates after 5 minutes under sunlight, changes blue-tinted transparent into by water white transparency, and sunlight transmittance reduces 30% than before illumination, and shading coefficient declines about 0.28, shows to have good shaded effects; Place 1 hour under no light condition, changed into again light blue transparent by blue-tinted transparent, sunlight transmittance rises 17% than after illumination, shading coefficient declines about 0.16, place under no light condition after 5 hours, to fade completely and sunlight transmittance returns to the vitreous state before illumination, show that this inorganic photochromic doubling glass has good performance of fading.
Embodiment of the present invention photochromic glass adopts in polyvinyl butyral acetal basement membrane and disperses organic photochromic powder, do not change the basic structure of existing laminated glass, drop into lower, but there is efficient color changeable effect, due to employing is metal oxide, nontoxic environmental protection, nonflammable, security is high, meets the demand of current energy-saving and emission-reduction, the preparation method of above-mentioned photochromic glass, on can not change original preparation technology, preparation technology is simple, and cost is low, is applicable to building glass and the field such as automobile skylight glass, side window glass.
Below in conjunction with specific embodiment, above-mentioned photo chromic glass preparation method is described in detail.
Embodiment one
The present embodiment photochromic glass preparation method, comprises the steps:
The first step, the photochromic film of preparation PVB:
Get the polyvinyl butyral acetal of 85 weight percents, the two positive heptanoate of triglycol of 13.5 weight percents, the vinyltriethoxysilane of 1.15 weight percents and 0.35 weight percent spiropyran organic photochromic powder, after Homogeneous phase mixing, be added in mixing roll and stir 10 minutes, be heated to 150 DEG C of meltings and extrude and make film, after by operations such as cooling, anhydrate, dry up, obtain photochromic film;
Second step, prepare photochromic doubling glass:
Between two sheet glass of surface clean, clamp a photochromic film prepared with the step 2 of homalographic, to put in the lump in silica gel bag and be vented 20 minutes under 2.5KPa vacuum tightness and transfer in drying oven 85 DEG C of insulations 30 minutes; Then, in autoclave, at 1.3MPa pressure and 135 DEG C, hot pressing 25 minutes, obtains photochromic glass.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a photochromic film, is characterized in that, comprises the component of following weight percent:
Described organic photochromic powder is selected from spiropyran and derivative thereof, acyl for more than one of aniline, schiff bases or osazone;
Described softening agent be selected from the two positive heptanoate of triglycol, triglycol two 2-ethylhexoate more than one;
Described coupling agent be selected from vinyltriethoxysilane, 3-methacryloxypropyl trimethoxy silane coupling agent, hexanediamine ylmethyl triethoxyl silane, γ-aminopropyl triethoxysilane more than one.
2. photochromic film as claimed in claim 1, is characterized in that, the thickness of described photochromic film is 0.38 ~ 3.04 millimeter.
3. a photochromic glass, it is characterized in that, comprise the first mutually stacked glass coating, the second glass coating, the first PVB layer, the second PVB layer and photochromic film according to claim 1, described first PVB layer, the second PVB layer are stacked to be incorporated between described first glass coating and the second glass coating, and described photochromic film is stacked to be combined between the first PVB layer, the second PVB layer.
4. photochromic glass as claimed in claim 3, it is characterized in that, the thickness of described photochromic film is 0.38 ~ 3.04 millimeter.
5. a photochromic glass preparation method, comprises the steps:
Photochromic film described in first glass coating, the second glass coating, the first PVB layer, the second PVB layer and right 1 or 2 is provided;
By described first PVB layer, the second PVB layer is stacked is incorporated between described first glass coating and the second glass coating, described photochromic film layers is stacked between the first PVB layer, the second PVB layer, obtains photochromic glass through hot pressing.
6. photochromic glass preparation method as claimed in claim 5, it is characterized in that, described hot pressing temperature is 110 ~ 150 DEG C, and pressure is 1.0 ~ 3MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI558679B (en) * | 2015-11-18 | 2016-11-21 | 東元奈米應材股份有限公司 | A manufacture method of a sandwich glass and the sandwich glass thereof |
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| CN104059554B (en) * | 2014-06-12 | 2017-06-27 | 浙江德斯泰新材料股份有限公司 | Temperature sense discoloration polyvinyl butyral resin intermediate coat and preparation method thereof |
| CN104299511B (en) * | 2014-10-28 | 2017-03-22 | 东北林业大学 | Application of reversible photochromic wood anti-counterfeit label |
| CN105129225B (en) * | 2015-07-17 | 2018-01-02 | 东莞市纳利光学材料有限公司 | A kind of photochromic diaphragm and manufacture method |
| CN106739611A (en) * | 2016-12-05 | 2017-05-31 | 天津市瑞擎影像材料有限公司 | A kind of waterproofing protection film of new medical aseptic dressing |
| CN108913062A (en) * | 2018-05-24 | 2018-11-30 | 合肥学院 | A kind of photosensitive colour-changing environmental protection type sealing adhesive and preparation method thereof |
| CN113448005B (en) * | 2021-06-29 | 2022-12-02 | 江西沃格光电股份有限公司 | Optical composite film, preparation method and application thereof and display device |
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| US6916537B2 (en) * | 2001-11-01 | 2005-07-12 | Transitions Optical Inc. | Articles having a photochromic polymeric coating |
| CN202147451U (en) * | 2011-06-27 | 2012-02-22 | 浙江鼎昇新材料科技有限公司 | Photochromic glass |
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| TWI558679B (en) * | 2015-11-18 | 2016-11-21 | 東元奈米應材股份有限公司 | A manufacture method of a sandwich glass and the sandwich glass thereof |
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