CN108102106B - Photochromic cellulose and preparation method thereof - Google Patents
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Abstract
The invention discloses a photochromic cellulose and a preparation method thereof, wherein the preparation raw materials of the photochromic cellulose comprise, by mass, 0.01-10 parts of cellulose, 10-1000 parts of organic photochromic ligand solution and 5-2000 parts of metal ion solution; the organic photochromic ligand solution is prepared by mixing an organic photochromic ligand and an organic solvent according to a mass ratio of 1: (20-100) preparing; the metal ion solution is prepared by mixing a metal center and an organic solvent according to a mass ratio of 1: (10-20) preparation.
Description
Technical Field
The invention belongs to the field of cellulose preparation, and particularly relates to photochromic cellulose and a preparation method thereof.
Background
The inorganic photochromic material has the advantages of fatigue resistance, easy processing and high response speed. But the stability is poor and the structural form is single. The MOFs is a crystalline porous material with a periodic network structure formed by connecting inorganic metal centers (metal ions or metal clusters) and organic ligands which are bridged by self-assembly. Such photochromic materials have received wide attention in fields such as anti-counterfeiting coatings, photochromic glasses and lens applications because of their remarkable color change effects.
Disclosure of Invention
The invention aims to find an organic photochromic ligand with a redox center having strong absorption or high quantum yield in a visible light region, namely, the purpose of photochromism is achieved by constructing a photochromic group in MOFs, and a novel photochromic material is provided.
In order to achieve the purpose, the invention adopts the following technical scheme:
the photochromic cellulose is prepared from 0.01-10 parts by mass of cellulose, 10-1000 parts by mass of organic photochromic ligand solution and 5-2000 parts by mass of metal ion solution;
the organic photochromic ligand solution is prepared by mixing an organic photochromic ligand and an organic solvent according to a mass ratio of 1: (20-100) preparing;
the metal ion solution is prepared by mixing a metal center and an organic solvent according to a mass ratio of 1: (10-20) preparation.
Further, the cellulose is one or more of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose and microcrystalline cellulose.
Further, the metal center is one or more of zinc nitrate hexahydrate, zinc nitrate tetrahydrate, zinc nitrate, chromium nitrate or copper acetate;
the organic photochromic ligand is one or more of the following;
the organic solvent is one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone or absolute ethyl alcohol.
The preparation method of the photochromic cellulose comprises the following steps:
1) dissolving an organic ligand in an organic solvent to prepare an organic ligand solution, adding cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving a metal center in an organic solvent, and stirring until the metal center is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, synthesizing metal ions and an organic photochromic ligand on cellulose in situ by an in-situ synthesis method to obtain a compound of the cellulose and a metal-organic framework compound, filtering, washing for a plurality of times by using an organic solvent, and drying to obtain the photochromic cellulose.
Further, the stirring temperature in the step 2) is 0-120 ℃, and the stirring speed is 5-7000 r/min.
Further, the temperature in the step 3) is increased to specifically the temperature which is required to be between room temperature and 120 ℃; the pressurizing is specifically carried out under the pressure requirement of 0.1-5.0 MPa.
Further, the reaction time in the step 3) is 4-24 h.
Further, the washing times in the step 3) are 2-10 times, and the drying temperature is 85-105 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
in the invention, the organic photochromic ligand, the metal center and the cellulose are combined at one time, so that the preparation process is simplified, the preparation energy consumption is reduced, and a novel high-efficiency photochromic cellulose is developed. The zinc nitrate hydrate and the organic photochromic ligand are dissolved in the organic solvent, so that the compatibility of the zinc nitrate hydrate and the organic photochromic ligand is improved, and the final product has excellent adsorbability; the cellulose, the ligand and the organic solvent are mutually dispersed, so that good contact between the cellulose and the ligand can be ensured.
During preparation, the preparation process of the photochromic cellulose comprises three modes of temperature rise, pressurization and combined temperature rise/pressurization; the heating or pressurizing mode can enable the combination between the organic photochromic ligand and the metal organic framework compound formed by the metal center and the fiber to be as fast as possible, and the trans-form of the heating/pressurizing combination can further promote the reaction to be faster; the bonding means between the metal organic framework compound and the fibers include: non-covalent bonds (ester bonds (-COO-), ether bonds (-O-), amino groups (-NH-), carbon-nitrogen bonds (-C-N-), and coordination bonds of Zn and the organic photochromic ligand, wherein the combination of the non-covalent bonds and the coordination bonds enables the non-covalent bonds and the coordination bonds to be more compact, and the method can be more suitable for the requirements of special industries.
Drawings
Fig. 1 is an XRD image of photochromic cellulose of example 1;
FIG. 2 is an SEM image of photochromic cellulose of example 1;
fig. 3 is an image of color change before and after light irradiation of the photochromic cellulose of example 1.
Detailed Description
Embodiments of the invention are described in further detail below:
the photochromic cellulose is prepared from 0.01-10 parts by weight of cellulose, 0.1-100 parts by weight of organic photochromic ligand solution and 5-2000 parts by weight of metal ion solution. The types and contents of cellulose are shown in table 1:
TABLE 1 cellulose types and contents
The components and contents of the organic photochromic ligand solution are shown in table 2:
TABLE 2 Components and amounts of organic photochromic ligand solutions
Wherein, the organic photochromic ligand is specifically shown as follows:
the components and contents of the metal ion solution are shown in table 3:
TABLE 3 composition and content of Metal ion solution
A preparation method of photochromic cellulose comprises the following steps:
1) dissolving an organic ligand in an organic solvent to prepare an organic ligand solution, adding cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving a metal center in an organic solvent, and stirring until the metal center is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, and synthesizing metal ions and an organic photochromic ligand on cellulose in situ by an in-situ synthesis method to obtain a compound of the cellulose and a metal-organic framework compound; then filtering, washing for a plurality of times by using an organic solvent, and drying to obtain the photochromic cellulose.
The present invention is described in further detail below with reference to examples:
example 1
1) Dissolving 0.5 part of ligand 1 in 10 parts of N, N-dimethylformamide to prepare an organic ligand solution, adding 0.01 part of cellulose nanowhisker into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 0.45 part of zinc nitrate hexahydrate in 5 parts of N, N-dimethylformamide, and stirring at the stirring speed of 5 revolutions per minute and the stirring temperature of 0 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction vessel, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.1MPa, the reaction is carried out for 4h, and the metal ions and the organic photochromic ligand are synthesized on the cellulose nanowhisker in situ by an in-situ synthesis method. Obtaining the compound of the cellulose nanowhisker and the metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 2 times by using N, N-dimethylformamide, and drying the washed mixture at 85 ℃ to obtain the photochromic cellulose.
As shown in the XRD pattern of the photochromic specialty paper of fig. 1, the absorption peak at 2 θ ═ 16.5 ° is a characteristic absorption peak of the metal-organic framework compound, and 2 θ ═ 22.37 ° and 34.5 ° are characteristic absorption peaks of cellulose. Indicating that the cellulose and the photochromic metal-organic framework compound form a complex.
As shown in the figure 2 of the SEM, the metal organic framework compound is in a cubic block shape and is uniformly distributed on the surface of the cellulose, so that the cellulose is well coated.
As shown in fig. 3, the photochromic cellulose has a color change image before and after illumination, and the photochromic cellulose is dark brown before illumination; it turned yellow after uv irradiation. Indicating that the photochromic cellulose has remarkable photochromic performance.
Example 2
1) Dissolving 4 parts of ligand 2 in 80 parts of absolute ethyl alcohol to prepare an organic ligand solution, adding 0.1 part of nano-cellulose crystal into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 4 parts of zinc nitrate tetrahydrate in 40 parts of absolute ethyl alcohol, and stirring at the stirring speed of 100 revolutions per minute and the stirring temperature of 25 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.2MPa, the reaction is carried out for 8 hours, and the metal ions and the organic photochromic ligand are synthesized on the nano-cellulose crystal in situ by an in-situ synthesis method. Obtaining the compound of the nano-cellulose crystal and the metal organic framework compound. Then filtering with a glass filter, washing with absolute ethyl alcohol for 3 times, and drying at 90 ℃ to obtain the photochromic cellulose.
Example 3
1) Dissolving 5 parts of ligand 3 in 100 parts of N, N-dimethylacetamide to prepare an organic ligand solution, adding 1 part of bacterial nano-cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 10 parts of zinc nitrate in 200 parts of absolute ethyl alcohol, and stirring at the stirring speed of 300 revolutions per minute and the stirring temperature of 35 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.25MPa, the reaction lasts for 10 hours, and the metal ions and the organic photochromic ligand are synthesized on the bacterial nano-cellulose in situ by an in-situ synthesis method. Obtaining the compound of the bacterial nano-cellulose and the metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 4 times by using absolute ethyl alcohol, and drying the washed mixture at 90 ℃ to obtain the photochromic cellulose.
Example 4
1) Dissolving 6 parts of ligand 4 in 150 parts of N, N-dimethylacetamide to prepare an organic ligand solution, adding 2 parts of microfibrillated cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 15 parts of zinc nitrate in 300 parts of N, N-dimethylacetamide, and stirring at a stirring speed of 700 revolutions per minute and a stirring temperature of 45 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.3MPa, the reaction is carried out for 12h, and the metal ions and the organic photochromic ligand are synthesized on the microfibrillated cellulose in situ by an in-situ synthesis method. Obtaining the compound of microfibrillated cellulose and metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 4 times by using absolute ethyl alcohol, and drying the washed mixture at the temperature of 92 ℃ to obtain the photochromic cellulose.
Example 5
1) Dissolving 6 parts of ligand 5 in 200 parts of N, N-dimethylformamide and absolute ethyl alcohol to prepare an organic ligand solution, adding 3 parts of microcrystalline cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 20 parts of zinc nitrate in 400 parts of N, N-dimethylformamide and absolute ethyl alcohol, and stirring at the stirring speed of 1000 revolutions per minute and the stirring temperature of 50 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.35MPa, the reaction time is 14h, and the metal ions and the organic photochromic ligand are synthesized on the microcrystalline cellulose in situ by an in-situ synthesis method. Obtaining the compound of the microcrystalline cellulose and the metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 5 times by using absolute ethyl alcohol, and drying the washed mixture at 94 ℃ to obtain the photochromic cellulose.
Example 6
1) Dissolving 7 parts of ligand 6 in 350 parts of N, N-dimethylformamide to prepare an organic ligand solution, adding 5 parts of cellulose nanowhiskers, nanocellulose crystals and bacterial nanocellulose into the organic ligand solution, and uniformly dispersing by ultrasonic to obtain a precursor solution;
2) dissolving 40 parts of copper acetate in 400 parts of absolute ethyl alcohol, and stirring at a stirring speed of 2000 rpm and a stirring temperature of 50 ℃ until the copper acetate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.38MPa, the reaction is carried out for 16h, and the metal ions and the organic photochromic ligand are synthesized on the cellulose nanowhisker, the nanocellulose crystal and the bacterial nanocellulose in situ by an in-situ synthesis method. Obtaining the compound of the cellulose nanowhisker, the nanocellulose crystal, the bacterial nanocellulose and the metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 6 times by using absolute ethyl alcohol, and drying the washed mixture at 96 ℃ to obtain the photochromic cellulose.
Example 7
1) Dissolving 8 parts of ligand 7 in 400 parts of N, N-dimethylformamide to prepare an organic ligand solution, adding 6 parts of cellulose nanowhiskers and nanocellulose crystals into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 60 parts of zinc nitrate hexahydrate, zinc nitrate tetrahydrate and zinc nitrate in 600 parts of N, N-dimethylacetamide and absolute ethyl alcohol, and stirring at a stirring speed of 3000 revolutions per minute and a stirring temperature of 70 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.4MPa, the reaction is carried out for 18h, and the metal ions and the organic photochromic ligand are synthesized on the cellulose nanowhisker and the nanocellulose crystal in situ by an in-situ synthesis method. Obtaining the compound of the cellulose nanowhiskers, the nanocellulose crystals and the metal organic framework compound. Then filtering the mixture by using a glass filter, washing the mixture for 7 times by using absolute ethyl alcohol, and drying the washed mixture at 98 ℃ to obtain the photochromic cellulose.
Example 8
1) Dissolving 9 parts of ligand 8 in 900 parts of N, N-dimethylformamide, N-dimethylacetamide and absolute ethyl alcohol to prepare an organic ligand solution, adding 8 parts of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose and microcrystalline cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 80 parts of zinc nitrate hexahydrate, zinc nitrate tetrahydrate, zinc nitrate, chromium nitrate and copper acetate in 1600 parts of N, N-dimethylformamide, N-dimethylacetamide and absolute ethyl alcohol, and stirring at a stirring speed of 4000 revolutions per minute and a stirring temperature of 80 ℃ until the zinc nitrate hexahydrate, the zinc nitrate tetrahydrate, the chromium nitrate and the copper acetate are completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.44MPa, the reaction is carried out for 20 hours, and the metal ions and the organic photochromic ligand are synthesized on the cellulose nanowhisker, the nanocellulose crystal, the bacterial nanocellulose, the microfibrillated cellulose and the microcrystalline cellulose in situ by an in-situ synthesis method. Obtaining the compound of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose, microcrystalline cellulose and metal organic framework compounds. Then filtering with a glass filter, washing with absolute ethyl alcohol for 8 times, and drying at 100 ℃ to obtain the photochromic cellulose.
Example 9
1) 9.99995 parts of ligand 9 are dissolved in 990 parts of N, N-dimethylformamide to prepare an organic ligand solution, 10 parts of microcrystalline cellulose is added into the organic ligand solution, and the solution is uniformly dispersed by ultrasonic to obtain a precursor solution;
2) dissolving 100 parts of zinc nitrate hexahydrate in 00 parts of N, N-dimethylformamide, and stirring at the stirring speed of 5000 revolutions per minute and the stirring temperature of 100 ℃ until the zinc nitrate is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.46MPa, the reaction is carried out for 22h, and the metal ions and the organic photochromic ligand are synthesized on the microcrystalline cellulose in situ by an in-situ synthesis method. Obtaining the compound of the microcrystalline cellulose and the metal organic framework compound. Then filtering with a glass filter, washing with absolute ethyl alcohol for 9 times, and drying at 102 ℃ to obtain the photochromic cellulose.
Example 10
1) Dissolving 10 parts of ligand 1, ligand 2, ligand 3, ligand 4, ligand 5, ligand 6, ligand 7, ligand 8 and ligand 9 in 990 parts of N, N-dimethylformamide, N-dimethylacetamide and absolute ethanol to prepare an organic ligand solution, adding 10 parts of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose and microcrystalline cellulose into the organic ligand solution, and performing ultrasonic dispersion uniformly to obtain a precursor solution;
2) dissolving 100 parts of zinc nitrate hexahydrate, zinc nitrate tetrahydrate, zinc nitrate, chromium nitrate and copper acetate in 1900 parts of N, N-dimethylformamide, N-dimethylacetamide and absolute ethyl alcohol, and stirring at 7000 revolutions per minute at a stirring speed and at 105 ℃ until the zinc nitrate, the zinc nitrate tetrahydrate, the chromium nitrate and the copper acetate are completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, wherein the heating range is 25-120 ℃, the pressure is 0.5MPa, and the reaction time is 24 hours, and in-situ synthesizing the metal ions and the organic photochromic ligand on the cellulose nanowhisker, the nanocellulose crystal, the bacterial nanocellulose, the microfibrillated cellulose and the microcrystalline cellulose by an in-situ synthesis method. Obtaining the compound of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose, microcrystalline cellulose and metal organic framework compounds. Then filtering the mixture by using a glass filter, washing the mixture for 10 times by using absolute ethyl alcohol, and drying the washed mixture at 105 ℃ to obtain the photochromic cellulose.
The organic photochromic ligand in the embodiment can also be replaced by other organic photochromic ligand models provided by the invention, and other conditions are unchanged.
Claims (5)
1. A preparation method of photochromic cellulose comprises the following steps of preparing raw materials of 0.01-10 parts of cellulose, 10-1000 parts of organic photochromic ligand solution and 5-2000 parts of metal ion solution by mass parts; the organic photochromic ligand solution is prepared by mixing an organic photochromic ligand and an organic solvent according to a mass ratio of 1: (20-100) preparing; the metal ion solution is prepared by mixing a metal center and an organic solvent according to a mass ratio of 1: (10-20) preparing;
the cellulose is one or more of cellulose nanowhiskers, nanocellulose crystals, bacterial nanocellulose, microfibrillated cellulose and microcrystalline cellulose;
the metal center is one or more of zinc nitrate hexahydrate, zinc nitrate tetrahydrate, zinc nitrate, chromium nitrate or copper acetate;
the organic photochromic ligand is one or more of the following;
the organic solvent is one or more of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone or absolute ethyl alcohol;
the method is characterized by comprising the following steps:
1) dissolving an organic photochromic ligand in an organic solvent to prepare an organic photochromic ligand solution, adding cellulose into the organic photochromic ligand solution, and uniformly dispersing by ultrasonic to obtain a precursor solution;
2) dissolving a metal center in an organic solvent, and stirring until the metal center is completely dissolved to obtain a metal ion solution;
3) adding the metal ion solution obtained in the step 2) into the precursor solution obtained in the step 1), transferring the mixed solution into a reaction container, reacting in a heating/pressurizing combined mode, synthesizing metal ions and an organic photochromic ligand on cellulose in situ by an in-situ synthesis method to obtain a compound of the cellulose and a metal-organic framework compound, filtering, washing for a plurality of times by using an organic solvent, and drying to obtain the photochromic cellulose.
2. The method of claim 1, wherein the stirring temperature in step 2) is 0-120 ℃ and the stirring rate is 5-7000 rpm.
3. The method for preparing photochromic cellulose according to claim 1, wherein the temperature rise in the step 3) is specifically from room temperature to 120 ℃; the pressurizing is specifically carried out under the pressure requirement of 0.1-5.0 MPa.
4. The method for preparing photochromic cellulose according to claim 1, wherein the reaction time in step 3) is 4 to 24 hours.
5. The method for preparing photochromic cellulose according to claim 1, wherein the washing times in step 3) are 2 to 10 times, and the drying temperature is 85 to 105 ℃.
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| DE10039903A1 (en) * | 2000-08-16 | 2002-02-28 | Philipp Guetlich | Novel transition metal co-ordination compounds with heterocyclic-substituted bis-(thien-3-yl)perfluorocyclopoentene photochromic ligands are useful in the solid state at room temperature in e.g. opto-magnetic switches |
| JP2008031120A (en) * | 2006-07-31 | 2008-02-14 | Nara Institute Of Science & Technology | Rare earth complex and use thereof |
| CN102241971A (en) * | 2011-05-04 | 2011-11-16 | 宁波大学 | Fluorescent material with photochromic property and preparation method thereof |
| CN106220898A (en) * | 2016-08-27 | 2016-12-14 | 郭云琴 | A kind of electrochromism nano-cellulose composite and preparation method thereof |
| CN107417794A (en) * | 2017-05-22 | 2017-12-01 | 中山大学 | A kind of photochromic fibre element and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10039903A1 (en) * | 2000-08-16 | 2002-02-28 | Philipp Guetlich | Novel transition metal co-ordination compounds with heterocyclic-substituted bis-(thien-3-yl)perfluorocyclopoentene photochromic ligands are useful in the solid state at room temperature in e.g. opto-magnetic switches |
| JP2008031120A (en) * | 2006-07-31 | 2008-02-14 | Nara Institute Of Science & Technology | Rare earth complex and use thereof |
| CN102241971A (en) * | 2011-05-04 | 2011-11-16 | 宁波大学 | Fluorescent material with photochromic property and preparation method thereof |
| CN106220898A (en) * | 2016-08-27 | 2016-12-14 | 郭云琴 | A kind of electrochromism nano-cellulose composite and preparation method thereof |
| CN107417794A (en) * | 2017-05-22 | 2017-12-01 | 中山大学 | A kind of photochromic fibre element and preparation method thereof |
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