CN110551326A - Cellulose nanocrystal/titanium dioxide chiral nematic structure composite film and preparation method thereof - Google Patents
Cellulose nanocrystal/titanium dioxide chiral nematic structure composite film and preparation method thereof Download PDFInfo
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- CN110551326A CN110551326A CN201910782830.7A CN201910782830A CN110551326A CN 110551326 A CN110551326 A CN 110551326A CN 201910782830 A CN201910782830 A CN 201910782830A CN 110551326 A CN110551326 A CN 110551326A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The invention relates to a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film and a preparation method thereof, wherein the preparation method comprises the following steps: dissolving titanium dioxide precursor tetrabutyl titanate in ethanol, slowly dropping concentrated sulfuric acid into a cellulose nanocrystalline solution prepared by hydrolysis, and slowly and naturally drying at room temperature to prepare the cellulose nanocrystalline/titanium dioxide chiral nematic structure composite film, wherein the cellulose nanocrystalline is self-assembled into a chiral spiral structure in the film forming process, and the hydrolysate of tetrabutyl titanate is uniformly attached to the periphery of the cellulose nanocrystalline and participates in the self-assembly process together. The method for preparing the composite film with the chiral helical structure by the one-step method has the advantages of simple process, convenient operation, no need of additional equipment, little pollution to the environment and realization of macro preparation. The prepared composite film can be used for optical devices, humidity sensors, anti-counterfeiting materials and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembly, in particular to a method for preparing the cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by one step.
Background
Cellulose is a renewable resource abundant in nature, and in the fifties of the last century, R ä nby first reported the preparation of cellulose colloidal suspensions by controlled sulfuric acid catalyzed degradation of cellulose fibers, Battista obtained a batch preparation of microcrystalline cellulose from high quality wood pulp cellulose as a raw material, with hydrochloric acid assisted degradation and ultrasonic post-treatment, by sulfuric acid hydrolysis, it chemically reacted with hydroxyl groups on the cellulose surface, grafting negatively charged sulfonate groups on its surface, causing the whiskers to disperse completely and uniformly in water due to electrostatic repulsion.
In the prior art, the titanium dioxide material with the chiral structure can be prepared only by using the chiral template for multiple times and cannot be obtained in one step, and meanwhile, the titanium dioxide precursor is easy to hydrolyze, so that the preparation process is complex, and the cost in the synthesis process is greatly increased.
Disclosure of Invention
In order to solve the problems mentioned in the prior art, the invention provides a simple, easy, rapid and efficient method for preparing the cellulose nanocrystal/titanium dioxide chiral nematic structure composite film, and expands the way for preparing the nanocomposite.
The invention adopts the following technical scheme that a cellulose nanocrystalline/titanium dioxide chiral nematic structure composite film and a preparation method thereof, a titanium dioxide precursor is dissolved in solutions such as ethanol, the solutions are fully mixed and then slowly dropped into a cellulose nanocrystalline suspension, the mixture is uniformly stirred, injected into a polystyrene culture dish and dried, and the cellulose nanocrystalline/titanium dioxide chiral nematic structure composite film is obtained.
In a preferred embodiment of the present invention, the method specifically comprises the steps of:
Step 1: preparing cellulose nanocrystals, namely preparing a cellulose nanocrystal suspension by acidolysis with concentrated sulfuric acid;
Step 2: preparing a precursor stable solution, namely dissolving a titanium dioxide precursor in a solvent to obtain a precursor solution, and fully stirring to obtain a stable and uniform solution;
And step 3: preparation of mixed solution-slowly adding the precursor solution into the cellulose nanocrystal suspension by a metering pump;
And 4, step 4: film formation-slow evaporation drying to form a film.
In a preferred embodiment of the invention, the cellulose nanocrystals are obtained by acid hydrolysis with sulfuric acid, and the concentration is not too high or too low, preferably 2.7 to 3.5 wt%.
In a preferred embodiment of the invention, the cellulose nanocrystals should be used under acidic conditions, with a pH between 4 and 6.
in a preferred embodiment of the invention, the titanium dioxide precursor is selected from tetrabutyl titanate.
In a preferred embodiment of the present invention, the solvent is selected from one or more of ethanol, methanol, tert-butanol, and the like.
The invention also protects the cellulose nanocrystalline/titanium dioxide chiral nematic structure composite film prepared by the method.
Compared with the existing titanium dioxide material preparation technology, the self-assembly method for preparing the cellulose nanocrystal/titanium dioxide chiral nematic structure composite film has the following advantages:
(1) According to the invention, tetrabutyl titanate is used as a precursor, a cellulose nanocrystal solution prepared by mixing and acidolysis is prepared, and a hydrolysis product of tetrabutyl titanate enters a helical structure of the cellulose nanocrystal by utilizing the property that the cellulose nanocrystal can be self-assembled into the chiral helical structure, and finally the composite film with the chiral helical structure is prepared in one step by drying at room temperature.
(2) the invention has simple process, convenient operation, no need of additional equipment, small pollution to the environment and wide application prospect in the aspects of optical devices, humidity sensors, anti-counterfeiting materials and the like.
Drawings
The invention will be further described with reference to the accompanying drawings, which are only schematic illustrations and illustrations of the invention, and do not limit the scope of the invention.
Fig. 1 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 10wt% of tetrabutyl titanate and 90wt% of cellulose nanocrystals under the condition of pH =5 in example 1 of the present invention.
fig. 2 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 20wt% of tetrabutyl titanate and 80wt% of cellulose nanocrystals under the condition of pH =5 in example 2 of the present invention.
Fig. 3 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 30wt% of tetrabutyl titanate and 70wt% of cellulose nanocrystals under the condition of pH =5 in example 3 of the present invention.
Fig. 4 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 40wt% of tetrabutyl titanate and 60wt% of cellulose nanocrystals under the condition of pH =5 in example 4 of the present invention.
Fig. 5 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 50wt% of tetrabutyl titanate and 50wt% of cellulose nanocrystals under the condition of pH =5 in example 5 of the present invention.
fig. 6 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly of a suspension containing 10wt% of tetrabutyl titanate and 90wt% of cellulose nanocrystals under the condition of pH =4 in example 6 of the present invention.
Fig. 7 is a scanning electron microscope picture of a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film prepared by self-assembly at pH =6 from an aqueous suspension containing 10wt% tetrabutyl titanate and 90wt% cellulose nanocrystals according to example 7 of the present invention.
FIG. 8 is a chart of the UV-Vis spectra of the samples of example 1 of the present invention with increased humidity.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Example 1
the first embodiment of the invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 10w% of tetrabutyl titanate and 90w% of cellulose nanocrystals under the condition of pH = 5. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =5 with deionized water.
Step 2: preparation of precursor stable solution-10 mul of tetrabutyl titanate is dissolved in 5mL of ethanol solution to obtain precursor solution, and the precursor solution is fully stirred for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
And 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
Example 2
The second embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 20w% of tetrabutyl titanate and 80w% of cellulose nanocrystals under the condition of pH = 5. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =5 with deionized water.
step 2: preparation of precursor stable solution-dissolving 25 mul of tetrabutyl titanate in 5mL of ethanol solution to obtain precursor solution, and fully stirring for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
And 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
example 3
The third embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 30w% of tetrabutyl titanate and 70w% of cellulose nanocrystals under the condition of pH = 5. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =5 with deionized water.
step 2: preparation of precursor stable solution-50 mul of tetrabutyl titanate is dissolved in 5mL of ethanol solution to obtain precursor solution, and the precursor solution is fully stirred for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
and 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
Example 4
the fourth embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 40w% of tetrabutyl titanate and 60w% of cellulose nanocrystals under the condition of pH = 5. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =5 with deionized water.
Step 2: preparation of precursor stable solution-75 mul tetrabutyl titanate is dissolved in 5mL ethanol solution to obtain precursor solution, and the precursor solution is fully stirred for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
And 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
Example 5
a fifth embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 50w% tetrabutyl titanate and 50w% cellulose nanocrystals at pH = 5. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =5 with deionized water.
Step 2: preparation of precursor stable solution-dissolving 100 mul of tetrabutyl titanate in 5mL of ethanol solution to obtain precursor solution, and fully stirring for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
And 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
example 6
A sixth embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 10wt% of tetrabutyl titanate and 90wt% of cellulose nanocrystals under the condition of pH = 4. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =4 with deionized water.
Step 2: preparation of precursor stable solution-10 mul of tetrabutyl titanate is dissolved in 5mL of ethanol solution to obtain precursor solution, and the precursor solution is fully stirred for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
and 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
Example 7
The seventh embodiment of the present invention provides a method for preparing a cellulose nanocrystal/titanium dioxide chiral nematic structure composite film by self-assembling a suspension containing 10wt% of tetrabutyl titanate and 90w% of cellulose nanocrystals under the condition of pH = 6. The method comprises the following steps:
Step 1: preparation of cellulose nanocrystals-64 wt% concentrated sulfuric acid acidolysis produced a cellulose nanocrystal suspension, which was formulated into a 3wt% solution with pH =6 by deionized water.
step 2: preparation of precursor stable solution-10 mul of tetrabutyl titanate is dissolved in 5mL of ethanol solution to obtain precursor solution, and the precursor solution is fully stirred for 2h to obtain stable and uniform solution.
And step 3: preparation of mixed solution-an ethanol solution of tetrabutyl titanate was added to 5g of the cellulose nanocrystal suspension by a metering pump at a dropping rate of 0.15mL/min, followed by stirring for 3 hours.
And 4, step 4: and (3) film formation, namely injecting 3mL of mixed solution into a polystyrene culture dish, and slowly drying for 48 hours at room temperature to obtain the composite film.
The scanning electron microscope pictures of the composite films prepared in the examples 1 to 7 are shown in the figures 1 to 7, and the one-step self-assembly method is a simple and efficient method for preparing the composite film with the chiral nematic structure. The sample from example 1 was used directly for humidity response, as shown in fig. 8, and tested for increasing maximum reflection wavelength with increasing humidity.
The invention has been described in an illustrative manner, and it is to be understood that the invention is not limited in its implementation to the details of construction and to the arrangements of the components set forth in the description, but is capable of equivalent embodiments or modifications, such as combinations of features, divisions or repetitions, or application of the concepts and arrangements of the invention without modification in other applications, all without departing from the spirit and scope of the invention.
Claims (7)
1. A composite film with a chiral nematic structure of cellulose nanocrystals/titanium dioxide and a preparation method thereof are characterized in that a titanium dioxide precursor is dissolved in a solvent, a stable solution is formed by stirring, concentrated sulfuric acid is slowly dripped into a cellulose nanocrystal suspension prepared by acidolysis, hydrolysis products of tetrabutyl titanate are uniformly attached to the periphery of the cellulose nanocrystals, participate in the self-assembly process together, and are slowly dried to form the composite film with the chiral nematic structure.
2. The method according to claim 1, characterized in that it comprises in particular the steps of:
Step 1: preparing cellulose nanocrystals, namely preparing a cellulose nanocrystal suspension by acidolysis with concentrated sulfuric acid;
Step 2: preparing a precursor stable solution, namely dissolving a titanium dioxide precursor in a solvent to obtain a precursor solution, and fully stirring to obtain a stable and uniform solution;
And step 3: preparation of mixed solution-slowly adding precursor solution into cellulose nanocrystal suspension;
And 4, step 4: film formation-evaporation drying to form a film.
3. The method according to claim 1 or 2, wherein the concentration of cellulose nanocrystals is 0.5-10 wt%, preferably 2.7-3.5 wt%.
4. The method according to claim 1 or 2, wherein the cellulose nanocrystals are used under acidic conditions and have a pH between 4 and 6.
5. The method according to claim 1 or 2, characterized in that the titanium dioxide precursor is selected from tetrabutyl titanate.
6. The method according to claim 1 or 2, wherein the solvent is selected from one or more of ethanol, methanol, tert-butanol and the like.
7. The cellulose nanocrystalline/titanium dioxide chiral nematic structure composite film prepared by the method of any one of claims 1-6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113214517A (en) * | 2021-05-21 | 2021-08-06 | 南京信息工程大学 | Preparation method of patterned thin film |
| CN117659470A (en) * | 2023-12-08 | 2024-03-08 | 浙江中发薄膜有限公司 | High-transparency ultraviolet shielding film for vehicle window and preparation method thereof |
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| CN113214517A (en) * | 2021-05-21 | 2021-08-06 | 南京信息工程大学 | Preparation method of patterned thin film |
| CN117659470A (en) * | 2023-12-08 | 2024-03-08 | 浙江中发薄膜有限公司 | High-transparency ultraviolet shielding film for vehicle window and preparation method thereof |
| CN117659470B (en) * | 2023-12-08 | 2024-06-04 | 浙江中发薄膜有限公司 | High-transparency ultraviolet shielding film for vehicle window and preparation method thereof |
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Application publication date: 20191210 |