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Fluorescent oxidized nanocellulose thin film with adjustable light color and preparation method of fluorescent oxidized nanocellulose thin film

A nanocellulose and nanofiber technology, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as limiting the application of luminescent materials, and achieve the effects of rich sources, long fluorescence lifetime and high fluorescence efficiency

Inactive Publication Date: 2019-05-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In recent years, researchers at home and abroad have carried out a series of work in the field of luminescent materials, but most of the material substrates use petroleum-based polymers, which not only limits the application of luminescent materials in biomedicine and other fields, but also faces unavoidable energy problem

Method used

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  • Fluorescent oxidized nanocellulose thin film with adjustable light color and preparation method of fluorescent oxidized nanocellulose thin film
  • Fluorescent oxidized nanocellulose thin film with adjustable light color and preparation method of fluorescent oxidized nanocellulose thin film
  • Fluorescent oxidized nanocellulose thin film with adjustable light color and preparation method of fluorescent oxidized nanocellulose thin film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] S1, preparation of oxidized nanocellulose aqueous dispersion:

[0037] Ultrasonic disperse 1g of CNF powder in aqueous solution to form a CNF suspension, then add 0.016g of TEMPO and 0.100g of NaBr to the system, then gradually add 3mL of NaClO solution to start the oxidation reaction, and keep the reaction under ultrasonic conditions for continuous Stir for three hours, adjust the pH of the reaction system with NaOH solution throughout the process and maintain it at 10±1, add hydrochloric acid to adjust the pH to neutral after the stirring is completed, and repeatedly centrifuge the obtained mixed system and wash it with deionized water to remove the above. A filter cake was obtained from the supernatant, and the filter cake was re-dispersed ultrasonically in deionized water to prepare a 0.5 wt% aqueous dispersion of oxidized nanocellulose.

[0038] S2, preparing rare earth compound DMF solution

[0039] Mixed rare earth metal organic framework LnCl 3 ·6H 2 O ([Tb]=...

Embodiment 2

[0043] S1 is the same as embodiment 1

[0044] S2, preparing rare earth compound DMF solution

[0045] Mixed rare earth metal organic framework LnCl 3 ·6H 2 O ([Eu]=0.3mmol) and 1,3,5-benzenetricarboxylic acid (60mg, 0.3mmol) were respectively dissolved in DMF (10mL); the amount of 1,3,5-benzenetricarboxylic acid dissolved in the DMF solution 6mg / mL;

[0046] S3, take 2 mL of DMF-Eu prepared in S2 3+ Solution and 0.5wt% oxidized nanocellulose aqueous dispersion prepared by 10mL S1 were ultrasonically mixed and stirred at room temperature for 10min, stirred at room temperature for 0.8-1.2h, sealed in a 23mL tetrafluoroethylene-lined stainless steel autoclave, and self-pressurized at 60°C Heat for 7 days. Then, the reaction system was gradually cooled to room temperature at a rate of 15 °C / h. Use a glass sand core funnel to vacuum filter to remove the solvent, and vacuum dry to obtain the oxidized nanocellulose / rare earth compound composite fluorescent film with adjustable...

Embodiment 3

[0048] S1 is the same as embodiment 1

[0049] S2 mixed rare earth metal organic framework LnCl 3 ·6H 2 O ([Tb][Eu]=0.3mmol) and 1,3,5-benzenetricarboxylic acid (60mg, 0.3mmol) were respectively dissolved in DMF (10mL), and 1,3,5-benzenetricarboxylic acid was dissolved in the DMF solution The amount of formic acid is 6mg / mL;

[0050] S3, take 2mL of the rare earth compound DMF solution prepared by S2 (wherein Eu:Tb=1:1) and 10mL of the 0.5wt% oxidized nanocellulose aqueous dispersion prepared by S1, and ultrasonically mix and stir at room temperature for 10min, and stir at room temperature for 0.8-1.2 h, sealed in a 23mL tetrafluoroethylene-lined stainless steel autoclave, and heated at 60°C for 7 days under autopressure. Then, the reaction system was gradually cooled to room temperature at a rate of 15 °C / h. Use a glass sand core funnel to vacuum filter to remove the solvent, and vacuum dry to obtain the oxidized nanocellulose / rare earth compound composite fluorescent fil...

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Abstract

The invention discloses a preparation method of a fluorescent oxidized nanocellulose thin film with the adjustable light color. The preparation method comprises the steps: cellulose nanofibers (CNFs)are adopted as a raw material to be oxidized and dispersed firstly, and then oxidized nanocellulose aqueous dispersion liquid is obtained; then misch metal organic frameworks of LnCl3.6H2O and 1,3,5-benzene tricarbonic acid are dissolved in DMF, wherein Ln is Eu and Tb; the nanocellulose aqueous dispersion liquid prepared in the step S1 is dripped into a DMF solution to be evenly stirred; and a heating reaction is carried out under a sealed condition, then a reaction system is gradually cooled to the room temperature at the speed of 15 DEG C / h, subjected to suction filtration to remove a solvent and dried, and the fluorescent oxidized nanocellulose thin film with the adjustable light color is obtained. Through the coordination effect of carboxyl on oxidized nanocellulose and rare-earth metal ions, the hydrogen bond effect between oxidized nanocellulose fibrils, and the physical doping effect between the coordination effect and the hydrogen bond effect, stability of the material is improved; and the preparation method has wide application prospects in the fields of fluorescent falsification preventing, biosensors and fluorescent imaging.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a fluorescent oxidized nano-cellulose film with adjustable light color and a preparation method thereof. Background technique [0002] Cellulose is the most abundant natural organic polymer material on the earth. Cellulose I is a naturally occurring form of cellulose, and its annual output exceeds 7.5×1010t. It is widely distributed in higher plants. In addition, marine animals, Cellulose is also found in algae, bacteria, fungi and invertebrates. As the most widely sourced plant product in nature, cellulose has the great advantages of environmental friendliness and strong regeneration. Nanocellulose is made of natural cellulose through chemical pretreatment, enzyme treatment and mechanical grinding. It is a new type of natural polymer material with high crystallinity, high strength, high transparency, high specific surface area and low density. It is often use...

Claims

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Application Information

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IPC IPC(8): C08L1/04C08K5/00C08J5/18C09K11/06
Inventor 张召马宁宁李新平张茜雅宋发发
Owner SHAANXI UNIV OF SCI & TECH
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