CN113429638A - Method for preparing erasable rewritable medium with rapid color change and high cycle number - Google Patents
Method for preparing erasable rewritable medium with rapid color change and high cycle number Download PDFInfo
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- CN113429638A CN113429638A CN202110687284.6A CN202110687284A CN113429638A CN 113429638 A CN113429638 A CN 113429638A CN 202110687284 A CN202110687284 A CN 202110687284A CN 113429638 A CN113429638 A CN 113429638A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention provides a method for preparing erasable rewritable medium with rapid color change and high cycle number. The preparation method comprises the following steps: dissolving an organic matrix material in deionized water to obtain an organic matrix material aqueous solution; the organic matrix material is one or a mixture of more than two of agarose, polyvinyl alcohol or gelatin; fully dispersing the inorganic photochromic material into deionized water to obtain a photochromic material aqueous solution; adding an alcohol solvent and mixing uniformly to obtain a mixed solution; the inorganic photochromic material is one of bismuth oxybromide, bismuth oxychloride, tungsten trioxide, molybdenum trioxide or ammonium molybdate; uniformly mixing the mixed solution with an organic matrix material aqueous solution; pouring into a mould, and naturally cooling to room temperature to obtain the erasable rewritable medium. The preparation process is simple to operate and is suitable for large-scale industrial production; the obtained erasable and rewritable medium can change color rapidly, has excellent cycle performance, high flexibility and self-support, and has great advantages in practical application.
Description
Technical Field
The invention relates to a preparation method of an erasable rewritable medium with quick color change and high cycle number, belonging to the field of intelligent materials.
Background
The paper making technology is one of four inventions in China, since the invention of Chualen in Western Han, paper becomes the most main carrier of information, and the inheritance and development of human civilization are greatly promoted. With the rapid development of information technology, we live in a new media era and neglect the role of paper. In contrast, global paper consumption has doubled in the last 30 years, and most information for many businesses is still recorded on paper today. Unfortunately, most of the printing paper is not used effectively and is discarded after only one reading; this not only causes waste of resources but also causes serious environmental problems. The erasable and rewritable medium can be written repeatedly without extra ink for printing, and is an attractive substitute.
It has been observed from the 19 th century Fritsche that tetracene can change from yellow to colorless under the action of air and light, and then can recover yellow under the action of heat, and the phenomenon of photochromism is gradually valued by people. Since 1940, in order to clarify the mechanism of discoloration, i.e., the change of a compound during discoloration, the structural change of a substance after reaction, and the formation of an intermediate transition state, researchers have made a lot of studies and refer to such a phenomenon as photochromism (photochromism). The advent of photochromic materials has provided the opportunity for the development of erasable rewritable media that can be written on repeatedly and printed without the need for additional ink.
Wang Wen shou et al reported a titanium dioxide/methylene blue/water photochromic system, by adding high molecular material hydroxyethyl cellulose (HEC) in the titanium dioxide/methylene blue/water photochromic system, hydroxyl in the hydroxyethyl cellulose can be combined with-N (CH) in the molecular structure of methylene blue3)2Forming hydrogen bond action to achieve the effect of stabilizing the molecules. (references "W.Wang, M.Ye, L.He, Y.Yin, Nanocrystalline TiO2-catalyst photo spectrum Color Switching, Nano lett.14(2014) 1681-.
There are also some patent reports on photochromic erasable and rewritable media, for example, chinese patent CN107446146A discloses a hydrogel with photochromic properties. The preparation method comprises the following steps: (a) adding a cationic monomer of methacryloyloxyethyl trimethyl ammonium chloride, a chemical cross-linking agent of N, N, -methylene bisacrylamide, a hydrophilic monomer of acrylamide and an initiator of potassium persulfate into deionized water, and stirring until the cationic monomer of methacryloyloxyethyl trimethyl ammonium chloride, the chemical cross-linking agent of N, N, -methylene bisacrylamide, the hydrophilic monomer of acrylamide and the initiator of potassium persulfate are completely dissolved; then adding auxiliary agent tetramethyl ethylene diamine into the solution; filling the prepared solution into a mold, and then placing the mold in an oven at 30-40 ℃ for reaction for 1-3 h; cooling to room temperature after reaction to finally prepare the photochromic hydrogel precursor hydrogel; (b) and (c) soaking the precursor hydrogel prepared in the step (a) in an ammonium molybdate solution, slightly stirring, and taking out the hydrogel after soaking for 2-4 h to finally prepare the hydrogel with photochromic characteristics. The hydrogel prepared by the method has complicated steps, needs to be added with materials such as a cross-linking agent, an initiator and the like in the film forming process, is not environment-friendly enough, is easy to be cross-linked unevenly in the cross-linking process, and is not beneficial to large-scale production. Also, the hydrogel obtained is not excellent in color-changing property and recycling ability due to the synthesis method.
Disclosure of Invention
In view of the deficiencies of the prior art, the present invention provides a method for making an erasable rewritable medium that changes color rapidly and with a high cycle number. The preparation process is simple to operate and is suitable for large-scale industrial production; the obtained erasable and rewritable medium can change color rapidly, has excellent cycle performance, high flexibility and self-support, and has great advantages in practical application.
The technical scheme of the invention is as follows:
a method of making a fast-changing, high cycle times erasable rewritable medium comprising the steps of:
(1) dissolving an organic matrix material in deionized water to obtain an organic matrix material aqueous solution; the organic matrix material is one or a mixture of more than two of agarose, polyvinyl alcohol or gelatin;
(2) fully dispersing the inorganic photochromic material into deionized water to obtain a photochromic material aqueous solution; adding an alcohol solvent and mixing uniformly to obtain a mixed solution; the inorganic photochromic material is one of bismuth oxybromide, bismuth oxychloride, tungsten trioxide, molybdenum trioxide or ammonium molybdate;
(3) heating and uniformly mixing the mixed solution obtained in the step (2) and an organic matrix material aqueous solution; pouring into a mould, and naturally cooling to room temperature to obtain the erasable rewritable medium.
According to the present invention, the volume ratio of the mass of the organic matrix material to the deionized water in the step (1) is 1: (5-30) g/mL.
According to the invention, the dissolving temperature in the step (1) is preferably 80-120 ℃, and the dissolving time is preferably 0.5-1 h.
According to the invention, the volume ratio of the mass of the inorganic photochromic material in the step (2) to the deionized water is (20-35): 1 mg/mL.
According to the invention, the alcohol solvent in the step (2) is one or a mixture of two of ethylene glycol and glycerol; the volume ratio of the alcohol solvent to the deionized water is 1 (1-4).
According to the present invention, the mass ratio of the organic matrix material in the organic matrix material aqueous solution to the inorganic photochromic material in the mixed solution in the step (3) is preferably (1-9): 1.
According to the invention, the heating temperature in the step (3) is preferably 80-100 ℃ and the heating time is preferably 0.5-1 h.
According to the present invention, the material of the mold in the step (3) is preferably glass, methyl methacrylate or metal.
The invention has the technical characteristics that:
the invention adopts the compounding of inorganic photochromic material and organic matrix material to prepare an erasable and rewritable medium with rapid color change and high cycle number. The inorganic photochromic material fades under the irradiation of ultraviolet light and recovers in the oxidation of air. Since no organic dye is required to be added as a color developing unit, the aging resistance and chemical corrosion resistance of the erasable rewritable medium are greatly improved. The specific inorganic photochromic materials of the present invention do not exhibit significant decay during the color change process, and thus effectively increase the cycle performance of the erasable rewritable medium. The specific inorganic photochromic material can be tightly combined with the specific organic matrix material, so that the color recovery can be promoted by depending on the organic matrix material and the moisture in the material, and the problem of dye leakage which often occurs in organic dyes is avoided. In the film forming process, the organic matrix material selected by the invention has the characteristic of cooling film forming, no additional cross-linking agent and initiator are needed, the film forming is rapid, the flatness is high, simultaneously, the erasable and rewritable medium with large size can be prepared, the method is safe and environment-friendly, and the method is suitable for mass production. In the synthesis process, the glycol or the glycerol is added as the anti-freezing water-retaining agent, so that the problem of frequent dehydration of materials such as a gel film and the like is effectively reduced, the color recovery is promoted, and the service life is prolonged. Meanwhile, the specific organic matrix material has excellent flexibility and self-supporting capability, and because of the special film forming method, the erasable and rewritable medium contains abundant micron-sized holes, so that the transportation of air in the erasable and rewritable medium is promoted while the moisture is effectively kept, the cycle performance of the erasable and rewritable medium is greatly improved, and the practical application of the erasable and rewritable medium is facilitated.
The invention has the following beneficial effects:
1. the erasable and rewritable medium with quick color change and high cycle number is prepared by selecting specific inorganic photochromic materials, organic matrix materials and alcohol solvents. The raw materials of the invention exert mutual synergistic action, so that the obtained erasable rewritable medium has the performance of quick color change response and excellent cycle performance; the cycle life is long, the cycle times can reach more than 100, and the response speed and the color are not obviously attenuated in the cycle process.
2. The erasable and rewritable medium is prepared by utilizing the inorganic photochromic material which can change colors, an additional color development unit is not needed, the stability is good, the cost is low, the problems of damage and leakage of the color development unit are solved, the anti-aging and chemical erosion capabilities are high, and the practical value is high.
3. The erasable and rewritable medium prepared by the inorganic photochromic material has high flexibility and can be self-supported, and meanwhile, the large-size medium can be prepared due to the simple preparation process, can be flexibly used for short-term reading, display boards and other applications, and has great advantages in practical application.
4. The preparation process adopted by the invention is simple to operate, simple in material components, flexible and convenient in preparation process, safe and environment-friendly, and suitable for large-scale industrial production.
Drawings
FIG. 1 is an SEM image of the erasable rewritable medium prepared in example 1.
FIG. 2 is a digital photograph of the discoloration and recovery of the erasable rewritable medium prepared in example 1.
FIG. 3 is a graph of the UV-vis spectra of the erasable and rewritable medium prepared in example 1 at different UV exposure times; wherein the abscissa is wavelength and the ordinate is absorbance.
FIG. 4 is a graph of the UV-vis spectra in air at various times after discoloration of the erasable and rewritable medium prepared in example 1; wherein the abscissa is wavelength and the ordinate is absorbance.
FIG. 5 is a reversible color change cycle plot for the erasable rewritable medium prepared in example 1.
FIG. 6 is a graph of the effect of writing on the erasable rewritable medium prepared in example 1.
Fig. 7 is a graph of the effect of photo-printing using ultraviolet light on the erasable rewritable medium prepared in example 1.
Fig. 8 is a digital photograph and the effect of color change after 5 days of air exposure of the erasable rewritable medium prepared in comparative example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A method for preparing erasable rewritable medium with rapid color change and high cycle number comprises the following steps:
(1) dissolving 0.2g of agarose in 6mL of deionized water, and heating at 120 ℃ for 1h to obtain an agarose aqueous solution;
(2) dispersing 180mg of bismuth oxybromide material in 8.25mL of deionized water, adding 6mL of glycerol, and uniformly mixing;
(3) mixing the agarose aqueous solution obtained in the step (1) with the mixed solution obtained in the step (2), and stirring for 30 minutes at 100 ℃ to uniformly mix the agarose aqueous solution and the mixed solution;
(4) and (4) pouring the mixed solution obtained in the step (3) into a glass mold prepared in advance, and cooling to room temperature to obtain the erasable and rewritable medium.
SEM images of the erasable and rewritable media prepared in this example as shown in fig. 1, the erasable and rewritable media prepared in the present invention contains a large number of micro-scale pores inside, which facilitates air transportation in the erasable and rewritable media. The erasable and rewritable medium prepared by the embodiment can be changed into a brownish black colored state from white only by 60 seconds under the irradiation of ultraviolet light, and can be restored to a white faded state after being placed in the air for 15min, and a specific photo is shown in fig. 2. The erasable rewritable medium prepared by the embodiment has a UV-vis spectrum which changes color along with the irradiation of ultraviolet light, as shown in FIG. 3, only needs to be irradiated by the ultraviolet light for 60s from the original state that the whole body is white to the colored state that the deep coloring is brownish black, and has extremely high color change rate. Meanwhile, the UV-vis spectra of the erasable and rewritable medium prepared in this example at different times in the air after changing color are shown in fig. 4, wherein the original curve is the ultraviolet absorption curve in the brownish black colored state in fig. 2, because the erasable and rewritable medium has a structure capable of effectively retaining moisture while promoting the transportation of air, so that the inorganic photochromic material after changing color can be rapidly recovered, and the erasable and rewritable medium after changing color can be recovered to the original color after 15 minutes in the air. The erasable rewritable medium prepared in this example was subjected to UV-vis spectroscopy for reversible cyclic color change, and then the absorbance at 420nm of the absorption spectrum was taken to make a reversible cyclic graph, as shown in FIG. 5. It can be seen from fig. 5 that there is no significant attenuation after 100 cycles. Writing on the erasable and rewritable medium prepared in this example with an ultraviolet laser pen resulted in a very clear effect pattern as shown in fig. 6 and was recoverable in air. Meanwhile, the pre-designed template can be used for printing a required image on the erasable and rewritable medium by using ultraviolet light, and as shown in fig. 7, the printed image is very clear and has high practical value; and can be recovered in the air.
Example 2
A method for preparing erasable rewritable medium with rapid color change and high cycle number comprises the following steps:
(1) dissolving 0.2g of agarose in 6mL of deionized water, and heating at 120 ℃ for 1h to obtain an agarose aqueous solution;
(2) dispersing 180mg of ammonium molybdate material in 8.25mL of deionized water, adding 6mL of ethylene glycol, and uniformly mixing;
(3) mixing the agarose aqueous solution obtained in the step (1) with the mixed solution obtained in the step (2), and stirring for 30 minutes at 100 ℃ to uniformly mix the agarose aqueous solution and the mixed solution;
(4) and (4) pouring the mixed solution obtained in the step (3) into a glass mold prepared in advance, and cooling to room temperature to obtain the erasable and rewritable medium.
Example 3
A method for preparing erasable rewritable medium with rapid color change and high cycle number comprises the following steps:
(1) dissolving 1.0g of gelatin in 5mL of deionized water, and heating at 100 ℃ for 1h to obtain a gelatin aqueous solution;
(2) dispersing 120mg of bismuth oxybromide in 3.5mL of deionized water, adding 2mL of glycerol, and uniformly mixing;
(3) mixing the gelatin aqueous solution obtained in the step (1) with the mixed solution obtained in the step (2), and stirring for 30 minutes at 100 ℃ to uniformly mix the gelatin aqueous solution and the mixed solution;
(4) and (4) pouring the mixed solution obtained in the step (3) into a glass mold prepared in advance, and cooling to room temperature to obtain the erasable and rewritable medium.
Comparative example 1
An erasable rewritable medium was prepared in the same manner as in example 1 except that glycerin was not added in the step (2); the other steps and conditions were identical to those of example 1.
The erasable rewritable medium prepared by this comparative example was the same as the erasable rewritable medium of inventive example 1 with glycerol added for the first few days and was not significantly different. However, the erasable rewritable medium prepared in comparative example 1 became dry and lost flexibility after 5 days, while the discoloration and recovery effect were greatly reduced, as shown in fig. 8; whereas the erasable rewritable medium prepared in example 1 of the present invention showed no change in properties after being left for 5 days.
Comparative example 2
An erasable and rewritable medium was prepared in the same manner as in example 1, except that agarose, which is an organic base material added in the step (1), was replaced with acrylamide; the other steps and conditions were identical to those of example 1.
The erasable rewritable medium prepared by this comparative example was not film-forming by itself and was always liquid in the mold due to lack of effective crosslinking.
Comparative example 3
An erasable rewritable medium was prepared in the same manner as in example 1, except that the bismuth oxybromide added in step (2) was replaced with titanium dioxide; the other steps and conditions were identical to those of example 1.
The erasable rewritable medium prepared by the present comparative example was not discolored under the irradiation of ultraviolet light.
As is clear from comparison between comparative example 1 and example 1, the alcohol substance can effectively retain water as an anti-freeze water retention agent, forms strong hydrogen bonds with water molecules in the erasable and rewritable medium, competes with hydrogen bonds in water, destroys formation of ice crystal lattice at low temperature, prevents evaporation of water at high temperature, increases service time of the erasable and rewritable medium, and contributes to recycling. As can be seen from comparison of comparative example 2 and example 1, the erasable rewritable medium can be prepared by a natural cooling method without using materials such as a cross-linking agent, an initiator and the like, so that the method is convenient to operate, safe and environment-friendly. As is clear from comparison between comparative example 3 and example 1, the erasable rewritable medium is added with an inorganic photochromic material which can change color by itself, and a color developing unit is not needed, and materials which are commonly used in the past, such as titanium dioxide, tin dioxide and the like, can not change color by itself because of no color developing unit, so that the material can not change color under the irradiation of ultraviolet light.
Claims (8)
1. A method of making a fast-changing, high cycle times erasable rewritable medium comprising the steps of:
(1) dissolving an organic matrix material in deionized water to obtain an organic matrix material aqueous solution; the organic matrix material is one or a mixture of more than two of agarose, polyvinyl alcohol or gelatin;
(2) fully dispersing the inorganic photochromic material into deionized water to obtain a photochromic material aqueous solution; adding an alcohol solvent and mixing uniformly to obtain a mixed solution; the inorganic photochromic material is one of bismuth oxybromide, bismuth oxychloride, tungsten trioxide, molybdenum trioxide or ammonium molybdate;
(3) heating and uniformly mixing the mixed solution obtained in the step (2) and an organic matrix material aqueous solution; pouring into a mould, and naturally cooling to room temperature to obtain the erasable rewritable medium.
2. The method of claim 1 wherein the ratio of the mass of organic matrix material to the volume of deionized water in step (1) is 1: (5-30) g/mL.
3. The process for preparing a fast-changing, high cycle erasable rewritable medium according to claim 1, characterized in that the dissolution temperature in step (1) is 80-120 ℃ and the dissolution time is 0.5-1 h.
4. The method for preparing a fast-changing, high cycle erasable and rewritable medium according to claim 1, characterized in that the ratio of the mass of the inorganic photochromic material in step (2) to the volume of the deionized water is (20-35): 1 mg/mL.
5. The method for preparing a fast-changing, high cycle erasable and rewritable medium according to claim 1, wherein said alcohol solvent in step (2) is one or a mixture of ethylene glycol and glycerol; the volume ratio of the alcohol solvent to the deionized water is 1 (1-4).
6. The method for producing a fast-color-changing, high-cycle-number erasable rewritable medium according to claim 1, characterized in that the mass ratio of the organic base material in the organic base material aqueous solution and the inorganic photochromic material in the mixed solution in the step (3) is (1-9): 1.
7. The process for preparing a fast-changing, high cycle erasable rewritable medium according to claim 1, characterized in that the heating temperature in step (3) is 80-100 ℃ and the time is 0.5-1 h.
8. The method for preparing a fast-changing, high cycle erasable rewritable medium according to claim 1, wherein the mold in step (3) is made of glass, methylmethacrylate or metal.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115716939A (en) * | 2022-06-29 | 2023-02-28 | 湖南师范大学 | Sodium alginate-based ink-free photoetching printing paper capable of being repeatedly erased, dissolved and regenerated |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102693A (en) * | 2013-03-01 | 2013-05-15 | 新疆大学 | Preparation method of pyrazolone/gelatin-xanthan gum composite photochromic film |
| CN110684360A (en) * | 2018-07-04 | 2020-01-14 | 长春工业大学 | Preparation method of gelatin-based photochromic film for inkless printing |
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- 2021-06-21 CN CN202110687284.6A patent/CN113429638B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102693A (en) * | 2013-03-01 | 2013-05-15 | 新疆大学 | Preparation method of pyrazolone/gelatin-xanthan gum composite photochromic film |
| CN110684360A (en) * | 2018-07-04 | 2020-01-14 | 长春工业大学 | Preparation method of gelatin-based photochromic film for inkless printing |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115716939A (en) * | 2022-06-29 | 2023-02-28 | 湖南师范大学 | Sodium alginate-based ink-free photoetching printing paper capable of being repeatedly erased, dissolved and regenerated |
| CN115716939B (en) * | 2022-06-29 | 2024-01-26 | 湖南师范大学 | Sodium alginate-based ink-free photoetching printing paper capable of repeatedly erasing, writing, dissolving and regenerating |
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