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Preparation method of nano-cellulose aerogel and nano-cellulose aerogel

A nanocellulose and aerogel technology, which is applied in the field of nanocellulose aerogel and nanocellulose aerogel preparation, can solve the problem that it is difficult to control the smooth progress of the TEMPO oxidation of cellulose reaction process and the decline of the physical properties of the gel. and other problems, to achieve the effect of easy control, low density, and a wide range of sources

Active Publication Date: 2018-02-23
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of nano-cellulose airgel and nano-cellulose airgel, through the buffer solution to regulate the oxidation process and the addition of freeze-drying protective agent to solve the difficulty in controlling the oxidation of TEMPO in the prior art The smooth progress of the cellulose reaction process and the technical problems that lead to the decline in the physical properties of the gel during the later freeze-drying process

Method used

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  • Preparation method of nano-cellulose aerogel and nano-cellulose aerogel
  • Preparation method of nano-cellulose aerogel and nano-cellulose aerogel
  • Preparation method of nano-cellulose aerogel and nano-cellulose aerogel

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Embodiment 1

[0033] 1) Preparation of blank sample 1: soak the pulp (bleached coniferous wood pulp) in deionized water for 4 hours, disperse it for 15 minutes, prepare a pulp with a mass fraction of 10 wt%, and use a PFI refiner to refine the pulp. The beating degree is 70°-90°SR slurry; dissolve TEMPO and NaBr with distilled water, the amount of TEMPO is 0.01g / g, the amount of NaBr is 0.1g / g, and then mixed with the slurry; 10% NaClO is dissolved and diluted to 5%, The amount of NaClO is 0.5g / g, added dropwise, using NaOH solution to adjust the pH value dropwise, so that the pH value is kept at about 10.5, and the reaction time is controlled for about 1h. After 1h of reaction, a certain amount of ethanol is added to terminate the reaction; The oxidized cellulose suspension is dialyzed to neutral, suction filtered to form a filter cake, and after the moisture in the filter cake is measured, the filter cake is dissolved in deionized water to prepare a suspension slurry with a mass fraction o...

Embodiment 2

[0042] Preparation of sample 2: Preparation of sample 1: soak the pulp (bleached coniferous wood pulp) in deionized water for 4h, disintegrate for 15min, prepare a slurry with a mass fraction of 10wt%, and use a PFI refiner to refine the slurry , to obtain a beating degree of 70°-90°SR slurry; dissolve TEMPO and NaBr with distilled water, the amount of TEMPO is 0.01g / g, and the amount of NaBr is 0.1g / g, and then mixed with the slurry, and 10% NaClO is dissolved and diluted to 5 %, the amount of NaClO is 0.5g / g, added dropwise, using NaClO 2 CO 3 / NaHCO 3 The buffer solution is added dropwise to adjust the pH value, so that the pH value is kept at about 10.5, and the reaction time is controlled for about 1 hour. After 1 hour of reaction, a certain amount of ethanol is added to terminate the reaction; Filter into a filter cake, after measuring the moisture in the filter cake, dissolve the filter cake in deionized water, prepare a suspension slurry with a mass fraction of 1 wt%...

Embodiment 3

[0046] Preparation of Sample 3: Soak the slurry (bleached softwood pulp) in deionized water for 4h, disperse it for 15min, prepare a slurry with a mass fraction of 10wt%, and use a PFI refiner to refine the slurry to obtain a beating degree It is 70°-90°SR slurry; dissolve TEMPO and NaBr with distilled water, the dosage of TEMPO is 0.01g / g, the dosage of NaBr is 0.1g / g, then mix with the slurry, dissolve and dilute 10% NaClO to 5%, the dosage of NaClO 0.5g / g, added dropwise, using Na 2 CO 3 / NaHCO 3 The buffer solution is added dropwise to adjust the pH value, so that the pH value is kept at about 10.5, and the reaction time is controlled for about 1 hour. After 1 hour of reaction, a certain amount of ethanol is added to terminate the reaction; Filter into a filter cake, after measuring the moisture in the filter cake, dissolve the filter cake in deionized water, prepare a suspension slurry with a mass fraction of 1wt%, add 20% sorbitol with a quality of the absolute dry slu...

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Abstract

The invention relates to the technical field of preparation of cellulose aerogel and in particular relates to a preparation method of nano-cellulose aerogel and the nano-cellulose aerogel. The preparation method comprises the following steps: preparing nano-cellulose suspension by utilizing a TEMPO-mediated oxidation method, controlling the oxidation process through a buffer solution, adding a freeze-drying protective additive, performing high-pressure homogenization treatment and freeze drying, and treating, thereby obtaining the nano-cellulose aerogel. The nano-cellulose aerogel prepared bythe preparation method disclosed by the invention has the advantages of high strength, large specific surface area, low density, high porosity, uniform pore size distribution and the like. Moreover, the used freeze-drying protective additive is cheap, readily available, safe and non-toxic. Therefore, the prepared nano-cellulose aerogel does not have any toxicity or cause environmental pollution and is green and environmental-friendly.

Description

technical field [0001] The invention relates to the technical field of cellulose aerogel preparation, in particular to a preparation method of nano cellulose aerogel and the nano cellulose aerogel. Background technique [0002] Nanocellulose airgel uses cellulose as a raw material, and its raw material has a wide range of sources, is cheap and easy to obtain, and is a new type of environmentally friendly material. Because nanocellulose has a huge surface area, high hydrophilicity, high degree of polymerization, high Young's modulus, renewable and easy to degrade, and its chemical reactivity is much higher than that of cellulose, it can form stable colloidal solution. Since cellulose airgel is made of cellulose, it needs to dissolve the cellulose to form a gel, which will destroy the crystalline structure of cellulose and affect the strength of the airgel. [0003] Tetramethylpiperidine oxide, abbreviated as TEMPO, is a nitroxide free radical of piperidines. The TEMPO oxida...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08B15/02C08L1/04
CPCC08B15/02C08J9/28C08J2201/0484C08J2205/026C08J2301/04
Inventor 刘鹏涛侯佳玲惠岚峰刘忠
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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