Etherification and oxidization method for preparing cellulose nano crystal whiskers

A technology of nano-whiskers and cellulose, which is applied in the field of textile materials, can solve the problems of large size dispersion and low production rate of cellulose nano-whiskers, and achieve the effects of low cost, increased added value, and simple preparation process

Inactive Publication Date: 2015-07-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of etherification oxidation method for preparing cellulose nano-whiskers, solve plant fibers such as jute fiber, straw, cotton stalk skin because of low cellulose content that the cellulose nano-whiskers making rate is low, Problems such as large size dispersion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of etherification oxidation technology of preparing jute cellulose nano whisker, concrete steps are:

[0031] Step 1: Pretreatment: Clean the jute fibers with tap water and dry them in a vacuum oven at 60°C to constant weight. NaOH aqueous solution, the bath ratio is 1:20, after soaking for 24 hours, take it out and wash it, and dry it in a vacuum oven at 60°C to constant weight;

[0032] The second step: etherification treatment: the pretreated jute fiber is placed in a NaOH solution with a concentration of 60g / L, the bath ratio is 1:20, soaked at room temperature for 3h, then taken out, and the excess solution is thrown off with a centrifuge , and then placed in a reaction kettle for etherification reaction, the reaction process is: add propylene oxide with a weight of 0.2% of the dry weight of the fiber at 40°C, stir at 200rpm for 25min, then heat up to 70°C, and stir at 200rpm 120min; after the reaction is completed, take it out, neutralize the free base wit...

Embodiment 2

[0041] An etherification oxidation technology for preparing rice straw cellulose nano-whiskers, the specific steps are:

[0042] Step 1: Pretreatment: Wash the rice straw with tap water and dry it in a vacuum oven at 60°C until it reaches a constant weight. H 2 SO 4 In the aqueous solution, the bath ratio is 1:20, after soaking for 48 hours, take it out and wash it, and dry it in a vacuum oven at 60°C to constant weight;

[0043] The second step: etherification treatment: put the pretreated rice straw in a NaOH solution with a concentration of 100g / L, the bath ratio is 1:20, take it out after soaking at room temperature for 2 hours, and shake off the excess solution with a centrifuge , and then placed in a reaction kettle for etherification reaction, the reaction process is: add propylene oxide with a weight of 0.5% of the dry weight of the fiber at 40°C, stir at 300rpm for 20min, then heat up to 60°C, and stir at 300rpm 100min; take it out after the reaction is completed, ...

Embodiment 3

[0052] A kind of etherification oxidation technology of preparing corn bract cellulose nano-whiskers, the specific steps are:

[0053] The first step: pretreatment: wash the corn husks with tap water and dry them in a vacuum oven at 60°C to constant weight, and place them at a concentration of 100g / In NaOH aqueous solution of 1 L, the bath ratio is 1: 30, after soaking for 48 hours, take it out and wash it, and dry it in a vacuum oven at 60°C to constant weight;

[0054] The second step: etherification treatment: place the pretreated corn husks in a NaOH solution with a concentration of 80g / L, the bath ratio is 1:20, take it out after soaking at room temperature for 2 hours, and shake off the excess with a centrifuge solution, and then placed in a reaction kettle for etherification reaction, the reaction process is: add 0.4% propylene oxide with a weight of 0.4% of the dry weight of the fiber at 40°C, stir at a speed of 300rpm for 20min, then heat up to 60°C, and stir at a sp...

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Abstract

The invention provides an etherification and oxidization method for preparing cellulose nano crystal whiskers. The etherification and oxidization method is characterized by comprising the following steps: taking plant fibers with low cellulose content as raw materials; carrying out pre-treatment, etherification treatment and alkali treatment; carrying out mechanical crushing to obtain plant cellulose powder; carrying out TEMPO oxidization treatment, and stirring at a high speed to obtain a plant cellulose powder suspension solution; and carrying out centrifugal treatment, dispersion treatment, freezing and drying to prepare the cellulose nano crystal whiskers. The etherification and oxidization method has a simple preparation process, high yield and low energy consumption; in a production process, no toxic and harmless substances are discharged, and the method has a large-scale popularization and application potential; the used plant fibers can be jutes, straws, cotton stalk peels and the like, and have a wide raw material source and low cost; the environmental pollution problem is solved and the addition value of the plant fibers is also improved.

Description

technical field [0001] The invention relates to the etherification oxidation technology for preparing cellulose nano-whiskers, and belongs to the technical field of textile materials. Background technique [0002] Natural cellulose nano whiskers have been widely used because of their high strength, high modulus, good adsorption, and degradability. The current preparation methods mainly include: sulfuric acid acidification separation method, 2, 2, 6, 6-4 Methylpiperidinyl oxygen radical (TEMPO) ternary system oxidation separation method, mechanical method, etc., the former two are more commonly used. The sulfuric acid acidification separation method is based on the different resistance capabilities of the crystalline phase and the non-crystalline relative acid in cellulose. The non-crystalline phase is hydrolyzed first under acidic conditions, while the crystalline phase can maintain a relatively intact shape; the TEMPO oxidation separation method uses TEMPO / NaClO The / NaBr ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21B1/06D21B1/02D21C1/06C08B15/02C08B15/08C08B11/08
CPCC08B11/08C08B15/02C08B15/08D21B1/02D21C1/06
Inventor 刘丽芳李莉王晓婷刘慧赵艳娇俞子俊
Owner DONGHUA UNIV
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