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Preparation method of powder nano cellulose

A technology of nanocellulose and cellulose, applied in the field of preparation of powder nanocellulose, can solve the problems of harsh and cumbersome process, unsuitable for industrial production, serious agglomeration of nanocellulose, etc., and achieve the effect of mild reaction conditions

Inactive Publication Date: 2011-01-12
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the existing nanocellulose preparation technology, after the cellulose raw material is pretreated by different methods, it is hydrolyzed with various acids. Freeze-drying, the process is harsh and cumbersome, not suitable for industrial production; or the residual acid solution is neutralized by NaOH strong alkali, as a result, the nanocellulose obtained by drying is seriously agglomerated, and it is difficult to disperse into a colloid in water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 5 g of microcrystalline cellulose to 44 ml of 45% H 2 SO 4 Medium temperature, 40°C internal temperature, oil bath, magnetic stirring reaction for 5h, after cooling, add 250ml of distilled water to dilute to stop the reaction, let it stand, pour off the upper liquid, and filter the obtained solid mixture with NH 3 -NH 4 The Cl buffer solution was neutralized to pH = 7, washed twice with ethanol, centrifugally filtered, and dried to obtain a powdery solid. The powder was redispersed in water by ultrasonic waves to form a colloid. The length of the powder nanocellulose obtained in this example is 100-200nm , the width is 10-20nm.

Embodiment 2

[0023] After breaking the ashless filter paper with a pulverizer, pass through a 20-mesh sieve, weigh 10g and add it to 90ml of 65% H 2 SO 4 medium, heated in an oil bath, 45°C internal temperature, magnetic stirring for 1 h, added 900 ml of distilled water to dilute to stop the reaction, cooled to room temperature, left to stand, poured off the upper liquid, filtered with suction, added NH with pH=10 3 with NH 4 The Cl mixed buffer was neutralized to pH=7, washed twice with ethanol, centrifugally filtered, and dried to obtain a powdery solid, which was redispersed by adding water to the powdery solid to obtain a colloid. The length of the powdered nanocellulose obtained in this example was 100- 200nm, the width is 10-20nm.

Embodiment 3

[0025] Add 5 g of microcrystalline cellulose to 44 ml of 47% H 2 SO 4 Medium temperature, 45°C internal temperature, oil bath, magnetic stirring for 6h, adding 250ml of distilled water to dilute to stop the reaction, let it stand, pour off the upper liquid, filter with suction, and use Na 2 CO 3 with NaHCO 3 The mixed buffer was neutralized to pH=7, washed twice with ethanol, centrifugally filtered, and dried to obtain a powdery solid. The powder is re-dispersed by adding water to obtain a colloid. The nanocellulose powder obtained in this example has a length of 100-200 nm and a width of 10-20 nm.

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PUM

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Abstract

The invention discloses a preparation method of powder nano cellulose, comprising the following steps: hydrolyzing the cellulose with sulfuric acid; filtering the obtained mixture, and then introducing a buffer solution for neutralization until pH is equal to 7; and centrifugally filtering, rinsing and drying the neutralized mixture to obtain the powder nano cellulose. In the preparation method, acid liquor adsorbed by the nano cellulose is effectively neutralized and surface hydrogen bonds are damaged, thus the obtained powder nano cellulose is not agglomerate while being dried and can conveniently form stable colloid in water. The preparation method has the advantages of cheap and available buffer solution adopted in reaction and mild reaction condition, thus being applicable to industrial production.

Description

technical field [0001] The invention relates to a method for preparing materials, in particular to a method for preparing powder nanocellulose. Background technique [0002] The cellulose structure is a linear polymer formed by connecting D-glucopyranose rings to each other in a chair configuration with β-1,4-glycosidic bonds, and each ring has three hydroxyl groups (Angew.Chem.Int.Ed. 44, 3358-3393 (2005)). Nanocrystalline cellulose (nanocrystalline cellulose, NCC for short) refers to cellulose crystals with nanometer scale, its particle size is generally 30nm ~ 100nm, it has a huge specific surface area and the number of surface atoms, has a special surface effect, and still has The crystal form and properties of cellulose, the surface of nanocellulose is rich in hydroxyl groups, and there are a large number of intermolecular and intramolecular hydrogen bonds between the chains, which can easily cause agglomeration (Acta Polymer Sinica, 8, 982-986 (2006)), but nano The c...

Claims

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Application Information

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IPC IPC(8): C08J3/00C08J3/075C08L1/04C08B15/02
Inventor 王明亮陈立红陈娜周建成
Owner SOUTHEAST UNIV
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