CN105295108A - Preparation method for high-selectivity composite color film - Google Patents
Preparation method for high-selectivity composite color film Download PDFInfo
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- CN105295108A CN105295108A CN201410330020.5A CN201410330020A CN105295108A CN 105295108 A CN105295108 A CN 105295108A CN 201410330020 A CN201410330020 A CN 201410330020A CN 105295108 A CN105295108 A CN 105295108A
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Abstract
The invention discloses a preparation method for a high-selectivity composite color film. The preparation method is characterized by comprising the following steps: (1), preparation of graphene with a high specific surface area; (2), preparation of magnetic cellulose nanocrystals; (3), preparation of the composite color film: compounding the prepared nanocrystal suspension liquid with graphene, adding benzophenone as a photoinitiator, carrying out ultrasonic treatment and pressurizing to form the film. The water contents of the composite color film prepared by adding the benzophenone as the photoinitiator are different while the water immersion time of the color film is different, the reflected optical effects are different due to different water contents in the film, and the water content decides a special optical effect of wavelength light of the reflective film with selectivity, and the film can recover to the original color after being dried.
Description
Technical field
The invention belongs to technical field of film preparation, be specifically related to the preparation of colour film.
Background technology
Mierocrystalline cellulose is one of organism the abundantest on the earth, is inexhaustible, the nexhaustible renewable resources of nature.This product has the effects such as bonding, filling, film forming, for resins synthesis plastics, coating, rubber substitute, ink, insulating material, is also used as tackiness agent, textile finish etc.The application of cyanoethyl cellulose is very extensive, low DS(0.3 ~ 0.5) attack of mould and bacterium can be stoped, be applied in textiles.Partially substituted cyanoethyl cellulose heat resistanceheat resistant resistance to acid is fine, can avoid degraded.Cyanoethyl cellulose has high insulativity and can be used in isolator.Prior art is in preparation Cellulose nanocrystal, nobody adopts ethyl cellulose and cyanoethyl cellulose as raw material, and Cellulose nanocrystal size of the prior art is large, and its sepn process is more difficult, in conjunction with tight, skewness, limit its Application Areas.
In prior art, the Cellulose nanocrystal prepared of sulfuric acid solution is because sulfonate group on surface grafting, and special surface topography and contained a large amount of negative charges can be arranged in cholesteryl liquid crystal in aqueous, have the ability forming colour film.But the method length consuming time, needs the time of several days, the greatly speed of restriction film forming.Graphene as a kind of perfect Two-dimensional Carbon material because the conductivity of its excellence, optical property, mechanical property and resistance toheat are paid close attention to widely, also there is not report that Cellulose nanocrystal and Graphene compound are prepared carrying magnetic at present and there is the high method selecting colour film, therefore, how to produce carrying magnetic and there is high selection colour film, enhancing productivity, is the technical problem to be solved in the present invention.
Summary of the invention
Large for the Cellulose nanocrystal size existed in prior art, in conjunction with tight, skewness, and colour film preparation method length consuming time, the defects such as application effect of products is not remarkable, the object of the present invention is to provide the preparation method of the composite coloured film of a kind of highly selective.
The technical scheme that the present invention takes is:
A preparation method for the composite coloured film of highly selective, is characterized in that, specifically comprise the following steps:
(1) graphene with high specific surface processed: graphene oxide is immersed in alkaline electrolyte, with ultrasonic apparatus dispersion treatment 20-30min, solution lyophilize is obtained graphite oxide aerogel, and control voltage is between 80-120V, temperature is 240-250 DEG C, thermal reduction Graphene;
(2) magnetic cellulose nanocrystal processed: cellulosic material is added in acidic solution, regulate ph to 4-5, at 68-70 DEG C, acidolysis is carried out in stirring, add the ferrum sulfuricum oxydatum solutum that mass concentration is 0.08%, adding temperature is 90-100 DEG C of deionized water reaction 20-25min, centrifugation, by the washing of precipitate obtained, and repeated isolation to supernatant liquor becomes muddy;
(3) composite coloured film is made: the nanocrystal suspension prepared is diluted to 0.5 ~ 2wt%, according to Cellulose nanocrystal 99.0 ~ 99.7%, the part by weight of Graphene 0.3 ~ 1.0% carries out compound, the benzophenone adding Graphene weight 0.6-0.8% makes light trigger, supersound process 3-5h after mixing, control temperature is 38-40 DEG C, pressurization film forming.
Further, described step (1) neutral and alkali electrolytic solution is the mixture solution be made up of according to weight ratio 2:2:5 water glass, titanium dioxide and sodium hydroxide.
Further, in described step (2), acidic solution is the mixing solutions that sulfuric acid and hydrochloric acid form according to mol ratio 3:2.
Further, the mixture that in described step (2), cellulosic material adopts ethyl cellulose and cyanoethyl cellulose to form according to weight ratio 3:2.
Beneficial effect of the present invention is:
The first pre-treatment in alkaline electrolyte of Graphene in the present invention, the titanium in alkaline electrolyte, element silicon and Graphene combine, and for the color film in later stage improves titanium alloy surface hardness and wear resisting property, the specific surface area of the Graphene obtained by thermal reduction is high.
After cellulosic material acidolysis in the present invention, add ferric sulfate process, the Cellulose nanocrystal band of preparation is magnetic, and has that stronger selection is counter stings luminous energy power, and it has good stability again.
The composite coloured film of the present invention by Graphene and magnetic cellulose nanocrystal are obtained, preparation cycle is short, due under the existence of field of flow, shorten film formation time, obtained colour film smooth surface is smooth, and with metalluster, along with the changes colour of humidity also can change.
The obtained composite coloured film of light trigger is made by adding benzophenone, the color film water-immersed time is different, water content is different, in film, the difference of water content causes the optical effect difference reflected, how many decisions of water content have the special optical effect of the light of selective reflection wavelength, after film drying, original color can be recovered.
Embodiment
Embodiment 1
A preparation method for the composite coloured film of highly selective, is characterized in that, specifically comprise the following steps:
(1) graphene with high specific surface processed: graphene oxide is immersed in the alkaline electrolyte be made up of according to weight ratio 2:2:5 water glass, titanium dioxide and sodium hydroxide, with ultrasonic apparatus dispersion treatment 20min, solution lyophilize is obtained graphite oxide aerogel, control voltage is between 80V, temperature is 240 DEG C, and thermal reduction 20min obtains Graphene;
(2) magnetic cellulose nanocrystal processed: ethyl cellulose and cyanoethyl cellulose are added in the acidic solution that sulfuric acid and hydrochloric acid forms according to mol ratio 3:2 according to the cellulosic material that weight ratio 3:2 forms, regulate ph to 4-5, at 68 DEG C, acidolysis is carried out in stirring, add the ferrum sulfuricum oxydatum solutum that mass concentration is 0.08%, adding temperature is 100 DEG C of deionized water reaction 25min, centrifugation, by the washing of precipitate obtained, and repeated isolation to supernatant liquor becomes muddy;
(3) composite coloured film is made: the nanocrystal suspension prepared is diluted to 0.5wt%, compound is carried out according to Cellulose nanocrystal 30 milliliters and 0.9 milligram of Graphene ratio, the benzophenone adding Graphene weight 0.6% makes light trigger, supersound process 5h after mixing, control temperature is 38 DEG C, pressurization film forming.
Embodiment 2
A preparation method for the composite coloured film of highly selective, is characterized in that, specifically comprise the following steps:
(1) graphene with high specific surface processed: graphene oxide is immersed in the alkaline electrolyte be made up of according to weight ratio 2:2:5 water glass, titanium dioxide and sodium hydroxide, with ultrasonic apparatus dispersion treatment 25min, solution lyophilize is obtained graphite oxide aerogel, control voltage is between 100V, temperature is 245 DEG C, thermal reduction Graphene;
(2) magnetic cellulose nanocrystal processed: ethyl cellulose and cyanoethyl cellulose are added in the acidic solution that sulfuric acid and hydrochloric acid forms according to mol ratio 3:2 according to the cellulosic material that weight ratio 3:2 forms, regulate ph to 4-5, at 70 DEG C, acidolysis is carried out in stirring, add the ferrum sulfuricum oxydatum solutum that mass concentration is 0.08%, adding temperature is 100 DEG C of deionized water reaction 23min, centrifugation, by the washing of precipitate obtained, and repeated isolation to supernatant liquor becomes muddy;
(3) composite coloured film is made: the nanocrystal suspension prepared is diluted to 1wt%, compound is carried out according to Cellulose nanocrystal 30 milliliters and 0.9 milligram of Graphene ratio, the benzophenone adding Graphene weight 0.7% makes light trigger, supersound process 4h after mixing, control temperature is 40 DEG C, pressurization film forming.
Embodiment 3
A preparation method for the composite coloured film of highly selective, is characterized in that, specifically comprise the following steps:
(1) graphene with high specific surface processed: graphene oxide is immersed in the alkaline electrolyte be made up of according to weight ratio 2:2:5 water glass, titanium dioxide and sodium hydroxide, with ultrasonic apparatus dispersion treatment 30min, solution lyophilize is obtained graphite oxide aerogel, control voltage is between 120V, temperature is 250 DEG C, thermal reduction Graphene;
(2) magnetic cellulose nanocrystal processed: ethyl cellulose and cyanoethyl cellulose are added in the acidic solution that sulfuric acid and hydrochloric acid forms according to mol ratio 3:2 according to the cellulosic material that weight ratio 3:2 forms, regulate ph to 4-5, at 70 DEG C, acidolysis is carried out in stirring, add the ferrum sulfuricum oxydatum solutum that mass concentration is 0.08%, adding temperature is 100 DEG C of deionized water reaction 25min, centrifugation, by the washing of precipitate obtained, and repeated isolation to supernatant liquor becomes muddy;
(3) composite coloured film is made: the nanocrystal suspension prepared is diluted to 2wt%, compound is carried out according to Cellulose nanocrystal 30 milliliters and 0.9 milligram of Graphene ratio, the benzophenone adding Graphene weight 0.8% makes light trigger, supersound process 3h after mixing, control temperature is 40 DEG C, pressurization film forming.
Composite coloured film obtained by embodiment 1,2,3 is Graphene content is 0.5%, 1%, the composite solution of 2% colour film that the color that obtains of ultrasonic 3h, 4h, 4h is different respectively, this shows, the colour film of different colours can be obtained by the time controlling supersound process.By before colour film obtained in three embodiments immersion and place the photo of not time after being immersed in the water taking-up, can see that the color of colour film changes with the difference of water content in storage period and film, and after film drying, original color can be recovered, as can be seen here, the color of controlling diaphragm can be carried out by the water content controlling colour film.
Claims (4)
1. a preparation method for the composite coloured film of highly selective, is characterized in that, specifically comprise the following steps:
(1) graphene with high specific surface processed: graphene oxide is immersed in alkaline electrolyte, with ultrasonic apparatus dispersion treatment 20-30min, solution lyophilize is obtained graphite oxide aerogel, and control voltage is between 80-120V, temperature is 240-250 DEG C, thermal reduction Graphene;
(2) magnetic cellulose nanocrystal processed: cellulosic material is added in acidic solution, regulate ph to 4-5, at 68-70 DEG C, acidolysis is carried out in stirring, add the ferrum sulfuricum oxydatum solutum that mass concentration is 0.08%, adding temperature is 90-100 DEG C of deionized water reaction 20-25min, centrifugation, by the washing of precipitate obtained, and repeated isolation to supernatant liquor becomes muddy;
(3) composite coloured film is made: the nanocrystal suspension prepared is diluted to 0.5 ~ 2wt%, according to Cellulose nanocrystal 99.0 ~ 99.7%, the part by weight of Graphene 0.3 ~ 1.0% carries out compound, the benzophenone adding Graphene weight 0.6-0.8% makes light trigger, supersound process 3-5h after mixing, control temperature is 38-40 DEG C, pressurization film forming.
2. the preparation method of the composite coloured film of highly selective according to claim 1, is characterized in that, described step (1) neutral and alkali electrolytic solution is the mixture solution be made up of according to weight ratio 2:2:5 water glass, titanium dioxide and sodium hydroxide.
3. the preparation method of the composite coloured film of highly selective according to claim 1, is characterized in that, in described step (2), acidic solution is the mixing solutions that sulfuric acid and hydrochloric acid form according to mol ratio 3:2.
4. the preparation method of the composite coloured film of highly selective according to claim 1, is characterized in that, in described step (2), cellulosic material adopts the mixture that ethyl cellulose and cyanoethyl cellulose form according to weight ratio 3:2.
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| CN201410330020.5A CN105295108A (en) | 2014-07-12 | 2014-07-12 | Preparation method for high-selectivity composite color film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860143A (en) * | 2016-05-14 | 2016-08-17 | 上海大学 | Flexible nanocellulose-graphene composite membrane and preparation method thereof |
| CN107163298A (en) * | 2017-07-06 | 2017-09-15 | 东北林业大学 | A kind of chiral nematic nano-cellulose redox graphene laminated film and its preparation method and application |
-
2014
- 2014-07-12 CN CN201410330020.5A patent/CN105295108A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860143A (en) * | 2016-05-14 | 2016-08-17 | 上海大学 | Flexible nanocellulose-graphene composite membrane and preparation method thereof |
| CN107163298A (en) * | 2017-07-06 | 2017-09-15 | 东北林业大学 | A kind of chiral nematic nano-cellulose redox graphene laminated film and its preparation method and application |
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Application publication date: 20160203 |