Method for preparing nanocellulose at low energy consumption

A nano-cellulose and natural cellulose technology, applied in the field of cellulose derivatives, can solve the problems of organic solvent environmental pollution, high toxicity of chloroacetic acid, high equipment cost, etc., and achieve the effects of low environmental pollution, stable process and easy operation

Active Publication Date: 2015-07-08
桂林奇宏科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the oxidant used in the TEMPO oxidation method is more expensive, and precise control conditions are required at the same time; the toxicity of chloroacetic acid is relatively high; the environmental pollution of organic solvents in the reaction ball milling method and the high cost of equipment, etc.

Method used

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  • Method for preparing nanocellulose at low energy consumption
  • Method for preparing nanocellulose at low energy consumption
  • Method for preparing nanocellulose at low energy consumption

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Weigh 6 grams of sisal pulp and soak it with 18 ml of 5% sodium hydroxide aqueous solution at 20°C for 10 minutes to prepare a mixed solution.

[0021] (2) Take by weighing 0.55 gram of sodium hydroxide, mix it with 120 milliliters of ethanol and add it to the mixed solution prepared in step (1), under slow stirring, the reaction temperature is raised to 70°C; then add 1.85 gram of sodium chloroacetate, react 3 hours; then filtered, washed with distilled water to neutrality, and processed cellulose was obtained.

[0022] (3) adding the treated cellulose prepared in step (2) into 1000 milliliters of water to obtain a cellulose mixed solution, then shearing under high-speed stirring to form a gel, and finally diluting and centrifuging at a high speed, That is, the nanocellulose colloid is obtained.

[0023] The product that the present embodiment makes can obtain its productive rate by measuring and be 99.0%; The digital photo of prepared nanocellulose (taken through...

Embodiment 2

[0025] (1) Weigh 6 g of sisal pulp and soak it with 18 ml of 7.7% sodium hydroxide aqueous solution at 20°C for 10 minutes to obtain a mixed solution.

[0026] (2) Add 120 ml of ethanol to the mixed solution prepared in step (1), heat the reaction to 70°C under slow stirring; add 1.85 g of sodium chloroacetate, and react for 3 hours; then filter and wash with distilled water until neutral , to obtain the treated cellulose.

[0027] (3) Add the treated cellulose prepared in step (2) into 600 ml of water to obtain a cellulose mixture, then stir it into a gel with a high-pressure homogenizer, and finally dilute and separate it by high-speed centrifugation to obtain a cellulose mixture. Obtain transparent nanocellulose colloid.

[0028] The product that the present embodiment makes can obtain its productive rate by measuring and be 98.9%; The digital photo of prepared nanocellulose (taken through polarized light) sees figure 1 In (2), it can be seen that under polarized light, t...

Embodiment 3

[0030] (1) Weigh 3 g of sisal pulp and soak it with 9 ml of 15% sodium hydroxide aqueous solution at 10°C for 1 minute to prepare a mixed solution.

[0031] (2) Measure 43.9 milliliters of ethanol and join in the mixed solution that step (1) makes, under slow stirring, reaction is warmed up to 50 ℃; Then add 0.9 gram of sodium chloroacetate, react for 4 hours; Filter then, wash with distilled water until Neutral, the prepared cellulose.

[0032] (3) Add the treated cellulose prepared in step (2) into 200 ml of water, then shear it under high-speed stirring, and form a gel, and finally dilute and separate it by high-speed centrifugation to obtain nano-cellulose colloid .

[0033] The product that the present embodiment makes can obtain its productive rate by measuring and be 91.8%; The digital photo of prepared nanocellulose (taken through polarized light) sees figure 1 In (3), it can be seen that under polarized light, there is a light and dark image, indicating that the pre...

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Abstract

The invention discloses a method for preparing nanocellulose at low energy consumption. The method comprises the steps of soaking natural cellulose into a sodium hydroxide solution, and soaking at the temperature of 5-40 DEG C for 1-30 minutes to obtain a mixed solution; weighing sodium hydroxide and ethanol, and mixing sodium hydroxide and ethanol, then, adding the mixture into the mixed solution, heating the reactant to 50-78 DEG C while slowly stirring, then, adding sodium chloroacetate, reacting for 2.5-4 hours, then, filtering, and washing with distilled water until the solution is neutral to prepare treated cellulose; then, mixing the solution and water to prepare a cellulose mixed solution with the mass percentage of 0.5-1.4%; next, shearing under the mechanical action; and finally, filtering or carrying out centrifugal separation to prepare the nanocellulose. By using the method disclosed by the invention, the preparation time of the nanocellulose can be shortened to 3-4 hours, the yield is high, the consumption of a reaction reagent is low, the consumption of sodium chloroacetate is low, and the caused environment pollution is low; and the method is low in energy consumption, stable in process, good in repeatability, mild in condition, simple and convenient to operate and suitable for large-scale popularization.

Description

technical field [0001] The invention belongs to the technical field of cellulose derivatives, in particular to a method for preparing nano-cellulose with low energy consumption. Background technique [0002] Cellulose is the natural polymer material with the largest reserves. After continuous exploration and research, people have developed different types of derivatives and applied them in chemical industry, paint, food, cosmetics and other fields. Representative derivatives include carboxymethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose and the like. [0003] Nanocellulose is a natural plant fiber that can be obtained by mechanical methods [A.N.Nakagaito, et al. Appl.Phys.A78, 547-552 (2004)], chemical methods [Robert. , 40,3941-3994], mechanochemical method [Yong Huang, ChemSusChem 2012,5, 2319-2322] and other means obtained with high aspect ratio, high specific surface area, high strength (Young's modulus is about 110~220Gpa ), a nanomaterial with a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/12
Inventor 王世其韦春徐旭吕建
Owner 桂林奇宏科技有限公司
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