CN102219987A - Photochromic polyethylene terephthalate mixed film and preparation method thereof - Google Patents
Photochromic polyethylene terephthalate mixed film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a photochromic polyethylene terephthalate (PET) mixed film and a preparation method thereof. Specifically, a PET solution is dissolved into a suitable solvent to be blended with a photochromic material and a thin film is prepared by utilizing a solution film-forming method; the photochromic compound is basically not contacted with water and oxygen to effectively prevent from generating a degradation process so that the service life of the photochromic material is prolonged, the cost is reduced and the influence on each performance of the PET thin film is not great. The photochromic PET mixed film can be used for laminating external walls of top-grade buildings and exterior appearances of marked buildings and cars so that the wonderful colors of the city are increased and the environment is decorated and beautified; and the photochromic polyethylene terephthalate mixed film provided by the invention has a wide application prospect.
Description
Technical field
The present invention relates to a kind of mould material and preparation method thereof, more particularly, relate to a kind of photochromic polyethylene terephthalate hybrid films and preparation method thereof.
Background technology
Photochromic material was just reported to some extent as far back as 1867, but after Hirshberg proposition photochromic material in 1956 is applied to the possibility of optical recording storage, is just had received increasing attention.The photochromic compd A that is meant is when being subjected to wavelength and being the illumination of λ 1, can be by the specific chemical reaction generating structure product B different with spectrum property, and wavelength be λ 2 illumination or heat effect under, B reversibly generates the phenomenon of compd A again, its change procedure is shown below:
The essential characteristic of this process is: A, B under certain condition can both stable existences, and the color parallax is significantly different; Variation between A, the B is a reversible.
At present, photochromic research is mostly concentrated on diarylethene, fulgide, spiro-pyrans, Luo oxazine, azo class and the relevant heterogeneous ring compound, also continuing to explore and find new chromic systems simultaneously.It is mainly used in information storage element, decorates and the protective packaging material, and the autography holographic recording is taken a picture, and on the national defence, low but off-color material exists endurance, shortcomings such as bad mechanical property.
In order to improve the performances such as endurance of photochromic material, reduce old, make the application extension of photochromic material aspect the decoration protection, can attempt organic photochromic material and high molecular polymer are carried out blend, use the base carrier of superpolymer as photochromic material, utilize every good characteristic of superpolymer, aspects such as the endurance of off-color material, mechanical property, light transmission are improved, in the hope of making various aspects of performance good photochromic pad pasting.As people such as Yi Chen photochromic material and polarity PMMA are carried out solution blending and make the high film of a kind of transparency, the film variable color is obvious, excellent property.People such as Jeng-Shyong Lin carry out the solution blending film forming with photochromic material and SBS, but its film variable color is stable inadequately.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of preparation method who utilizes photochromic material to come modification polyethylene terephthalate (PET) film is provided, be some industries, provide a kind of attractive in appearance, practical pad pasting such as automobile industry, national defence industry etc.
Purpose of the present invention is achieved by following technical proposals:
The PET solid is dissolved in the solvent, wiring solution-forming, and carry out blend with photochromic material, adopt the solution film forming method to make film.
(1) dissolving of PET
Adopt multiple solvent, make the PET solution that concentration is 5%～10wt% as blend solution of mixed solution, butyl methacrylate, phenol and the tetrachloroethane of dimethyl formamide, dimethyl sulfoxide (DMSO), benzene and chlorobenzene etc., with standby.
(2) blend of PET, photochromic material
The light-induced variable toner is carried out the hand lapping refinement with mortar.Take by weighing an amount of light-induced variable toner, be added in a certain amount of PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with dusting cover.
(3) solution film forming
Sheet glass cleaned place in the baking oven constant temperature preheating temperature from room temperature to 100 ℃～260 ℃.Photochromic PET mixing solutions is cast on the sheet glass, puts into 100 ℃～260 ℃ baking oven constant temperature, treat to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
Polyethylene terephthalate (PET) is one of five large-engineering plastics varieties, has excellent comprehensive performances, oil resistant, anti-solvent, good fluidity, be easy to processing, wear resistance, thermotolerance, electrical insulating property and chemical proofing etc. are all very excellent, are widely used in synthetic terylen fiber and thin film fabrication, civilian blowing, can also be used for machinery, electronics, automobile, electrical equipment manufacturing and the consumer's goods as engineering plastics.The present invention is dissolved in PET solution in the suitable solvent, and carry out blend with photochromic material, adopt the solution film forming method to make film, photochromic compound is not contacted with oxygen with water basically, can effectively prevent the generation of degradation process, thereby it is prolonged the work-ing life of photochromic material, reduced cost, and little as every Effect on Performance of film to PET.The synthetic expansion for photochromic material of photochromic PET blend film is a significant development.This photochromic PET blend film can be used for top-grade building beyond the region of objective existence wall and sign property building and automobile appearance pad pasting, can increase the magical color in city, decorates and beautifies the environment, and is with a wide range of applications.
Description of drawings
Fig. 1 is a photochromic polyethylene terephthalate hybrid films of the present invention, and half that wherein is exposed in the light produced colour-change.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is to implement under the prerequisite in technical solution of the present invention, provided detailed embodiment and process, but protection domain of the present invention is not limited to following embodiment.
Embodiment 1
(1) the 5.0gPET solid is dissolved in makes 5% PET solution in the 95.0g solvent dimethylformamide.
(2) take by weighing the 0.025g photochromic material and carry out the hand lapping refinement with mortar.
(3) 0.025g light-induced variable toner is joined in 5% the PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with dusting cover.
(4) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 160 ℃.Not containing the pure solution casting of photochromic PET on sheet glass, natural curtain coating is put into 160 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming, treat that temperature is reduced to room temperature after, sheet glass is placed in the water soaks so that film and its disengaging.
(5) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 160 ℃.Photochromic PET mixing solutions is cast on the sheet glass, and natural curtain coating is put into 160 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
Embodiment 2
(1) the 6.0gPET solid is dissolved in makes 6% PET solution in the 94.0g dimethyl sulfoxide solvent.
(2) take by weighing the 0.06g photochromic material and carry out the hand lapping refinement with mortar.
(3) 0.06g light-induced variable toner is joined in 6% the PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with 200 order dusting covers.
(4) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 190 ℃.Not containing the pure solution casting of photochromic PET on sheet glass, natural curtain coating is put into 190 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming, treat that temperature is reduced to room temperature after, sheet glass is placed in the water soaks so that film and its disengaging.
(5) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 190 ℃.Photochromic PET mixing solutions is cast on the sheet glass, and natural curtain coating is put into 190 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
Embodiment 3
(1) the 7.0gPET solid is dissolved in the mixed solvent (volume ratio is 1: 1) of 80.5g benzene and chlorobenzene and makes 8.0% PET solution.
(2) take by weighing the 0.14g photochromic material and carry out the hand lapping refinement with mortar.
(3) 0.14g light-induced variable toner is joined in 8% the PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with 200 order dusting covers.
(4) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 180 ℃.Not containing the pure solution casting of photochromic PET on sheet glass, natural curtain coating is put into 180 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming, treat that temperature is reduced to room temperature after, sheet glass is placed in the water soaks so that film and its disengaging.
(5) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 180 ℃.Photochromic PET mixing solutions is cast on the sheet glass, and natural curtain coating is put into 180 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
Embodiment 4
(1) the 8.0gPET solid is dissolved in the mixed solvent (volume ratio is 1: 1) of 80.9g benzene and chlorobenzene and makes 9.0% PET solution.
(2) take by weighing the 0.24g photochromic material and carry out the hand lapping refinement with mortar.
(3) 0.24g light-induced variable toner is joined in 9% the PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with 200 order dusting covers.
(4) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 170 ℃.Not containing the pure solution casting of photochromic PET on sheet glass, natural curtain coating is put into 170 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming, treat that temperature is reduced to room temperature after, sheet glass is placed in the water soaks so that film and its disengaging.
(5) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 170 ℃.Photochromic PET mixing solutions is cast on the sheet glass, and natural curtain coating is put into 170 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
Embodiment 5
(1) the 10.0gPET solid is dissolved in the mixed solvent (volume ratio is 1: 1) of 80.9g phenol and tetrachloroethane and makes 10.0% PET solution.
(2) take by weighing the 0.4g photochromic material and carry out the hand lapping refinement with mortar.
(3) 0.4g light-induced variable toner is joined in 10% the PET solution, ultra-sonic dispersion is even, crosses elimination insoluble solid impurities wherein with 200 order dusting covers.
(4) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 200 ℃.Not containing the pure solution casting of photochromic PET on sheet glass, natural curtain coating is put into 200 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming, treat that temperature is reduced to room temperature after, sheet glass is placed in the water soaks so that film and its disengaging.
(5) sheet glass is cleaned placed in the baking oven constant temperature preheating temperature from room temperature to 200 ℃.Photochromic PET mixing solutions is cast on the sheet glass, and natural curtain coating is put into 200 ℃ baking oven constant temperature, treats to take out after the solvent evaporates film forming.Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above.Put into baking oven constant temperature, treat that solvent evaporates takes out after intact, treat that temperature reduces to room temperature, sheet glass is placed in the water soaks so that film and its disengaging.
Sample film to embodiment 1～5 preparation carries out property detection:
A. sample contrast before and after the variable color
Sample is cut into the batten of 5cm * 5cm, half shading, half illumination, viewing film colour-change.
B. mechanical property
Sample film is cut into the batten of 10mm * 100mm, and spacing jig is 20～50mm, and draw speed is 2～5mm/min, and calculation formula is:
Wherein P is the load of sample film fracture, N; D, b are the width and the thickness of sample, mm; L, L
0For sample when initial and two measuring lines during fracture between distance, mm.
C. thermal characteristics
At N
2Under the environment, the sample of 2～5mg earlier is heated to 80～140 ℃ with the speed of 10～20 ℃/min from room temperature and goes out moisture, is cooled to 10～30 ℃ and carries out melt temperature T again
mMeasure: temperature rise rate is 10～20 ℃/min, and sweep limit is 30～290 ℃.
D. the detection of photochromic properties
The test of the photochromic properties of sample utilizes 500W high pressure Hg lamp as the lamp source, sample when illumination with the distance of lamp source maintenance 6～30cm, the illumination process is at room temperature carried out in the air.Sample every 1min illumination once utilizes ultraviolet-visible pectrophotometer to measure its absorption peak strength.
E. water-intake rate
After sample film is cut into 5cm * 5cm, immerse in the distilled water, take out after 24 hours, carefully sop up to weigh behind the film surface-moisture with filter paper and obtain W
w, after being dried to constant weight under 45～100 ℃, weigh and obtain W
d, water-intake rate Q is calculated as follows:
Q＝(W
w-W
d)/W
d
W in the formula
w, W
dBe respectively the quality of wet film and dry film, kg.
The result shows: when the amount of photochromic material during at 0.5%～4.0wt%, film is obviously variable color under light conditions.Sample is cut into the batten of 5cm * 5cm, half shading, half illumination, the viewing film colour-change, as shown in Figure 1.The every Performance Detection that contains the different photochromic PET hybrid films of measuring is as shown in table 1.
Table 1: the every Performance Detection that contains the photochromic PET hybrid films of different amounts
From above data as can be seen, add the amount difference of photochromic material, every performance of PET hybrid films and pure PET film differ not too big, and adopt PET as base material, can also reduce cost, and improve photochromic endurance.As can be seen from the table, when the amount of photochromic material was 2.0%, it is best that the performance of PET hybrid films reaches.This adopts photochromic material and PET blend to prepare both artistic and practical film with regard to explanation is feasible.
More than the present invention has been done exemplary description; should be noted that; under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (9)
1. a photochromic polyethylene terephthalate hybrid films is characterized in that, the polyethylene terephthalate solid is dissolved in the solvent, and wiring solution-forming, and carry out blend with photochromic material, adopt the solution film forming method to make film.
2. a kind of photochromic polyethylene terephthalate hybrid films according to claim 1, it is characterized in that described solvent is the blend solution of mixed solution, butyl methacrylate, phenol and the tetrachloroethane of dimethyl formamide, dimethyl sulfoxide (DMSO), benzene and chlorobenzene.
3. a kind of photochromic polyethylene terephthalate hybrid films according to claim 1 is characterized in that the concentration that described polyethylene terephthalate solid is dissolved in wiring solution-forming in the solvent is 5%～10wt%.
4. a kind of photochromic polyethylene terephthalate hybrid films according to claim 1 is characterized in that the add-on of described photochromic material is 0.5%～4.0wt%.
5. the preparation method of a photochromic polyethylene terephthalate hybrid films is characterized in that, carries out according to following step:
(1) the polyethylene terephthalate solid is dissolved in the solvent wiring solution-forming;
(2) solution and the photochromic material that step (1) is made into carries out blend;
(3) adopt the solution film forming method to make film.
6. the preparation method of a kind of photochromic polyethylene terephthalate hybrid films according to claim 5, it is characterized in that the solvent of described step (1) is the blend solution of mixed solution, butyl methacrylate, phenol and the tetrachloroethane of dimethyl formamide, dimethyl sulfoxide (DMSO), benzene and chlorobenzene.
7. the preparation method of a kind of photochromic polyethylene terephthalate hybrid films according to claim 5 is characterized in that, the concentration that the polyethylene terephthalate solid of described step (1) is dissolved in wiring solution-forming in the solvent is 5%～10wt%.
8. the preparation method of a kind of photochromic polyethylene terephthalate hybrid films according to claim 5 is characterized in that, the add-on of photochromic material is 0.5%～4.0wt% in the described step (2).
9. the preparation method of a kind of photochromic polyethylene terephthalate hybrid films according to claim 5, it is characterized in that, in the described step (3), sheet glass cleaned place in the baking oven constant temperature preheating temperature from room temperature to 100 ℃～260 ℃, photochromic PET mixing solutions is cast on the sheet glass, put into 100 ℃～260 ℃ baking oven constant temperature, treat to take out after the solvent evaporates film forming; Pour into a mould the pure PET solution protective layer that one deck does not contain photochromic material after the drying more in the above; Put into baking oven constant temperature, treat that solvent evaporates is intact after, sheet glass is placed in the water soaks so that film and its disengaging.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102785441A (en) * | 2012-08-23 | 2012-11-21 | 东北林业大学 | Preparing method of photochromic composite films |
| CN102993613A (en) * | 2012-07-16 | 2013-03-27 | 上海甘田光学材料有限公司 | Photochromic material as well as preparation method and application of photochromic material |
| CN104962045A (en) * | 2015-06-13 | 2015-10-07 | 常州大学 | Photochromic ultraviolet-isolating heat-insulating window film |
| CN110511545A (en) * | 2019-09-18 | 2019-11-29 | 苏州宝丽迪材料科技股份有限公司 | The preparation method of photochromic fibre master batch |
| CN114277585A (en) * | 2021-12-09 | 2022-04-05 | 称意科技研发园(江苏)有限公司 | Method for dyeing polyester fabric by adopting diarylethene photochromic dye |
| CN114559688A (en) * | 2022-04-27 | 2022-05-31 | 河南银金达新材料股份有限公司 | Production process of durable photochromic PET (polyethylene terephthalate) film |
| CN114957758A (en) * | 2022-06-16 | 2022-08-30 | 电子科技大学广东电子信息工程研究院 | Negative photochromic film and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993613A (en) * | 2012-07-16 | 2013-03-27 | 上海甘田光学材料有限公司 | Photochromic material as well as preparation method and application of photochromic material |
| CN102785441A (en) * | 2012-08-23 | 2012-11-21 | 东北林业大学 | Preparing method of photochromic composite films |
| CN102785441B (en) * | 2012-08-23 | 2014-12-17 | 东北林业大学 | Preparing method of photochromic composite films |
| CN104962045A (en) * | 2015-06-13 | 2015-10-07 | 常州大学 | Photochromic ultraviolet-isolating heat-insulating window film |
| CN110511545A (en) * | 2019-09-18 | 2019-11-29 | 苏州宝丽迪材料科技股份有限公司 | The preparation method of photochromic fibre master batch |
| CN114277585A (en) * | 2021-12-09 | 2022-04-05 | 称意科技研发园(江苏)有限公司 | Method for dyeing polyester fabric by adopting diarylethene photochromic dye |
| CN114559688A (en) * | 2022-04-27 | 2022-05-31 | 河南银金达新材料股份有限公司 | Production process of durable photochromic PET (polyethylene terephthalate) film |
| CN114559688B (en) * | 2022-04-27 | 2022-07-29 | 河南银金达新材料股份有限公司 | Production process of durable photochromic PET (polyethylene terephthalate) film |
| CN114957758A (en) * | 2022-06-16 | 2022-08-30 | 电子科技大学广东电子信息工程研究院 | Negative photochromic film and preparation method and application thereof |
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Application publication date: 20111019 |