Method for producing NFC (nano-fibrillated cellulose)

A technology of cellulose and cellulase, applied in the fields of green chemistry and biomass energy and materials, can solve the problems of large consumption of TEMPO reagents, environmental pollution, high cost, etc., and achieve the effect of saving mechanical energy consumption

Inactive Publication Date: 2015-12-30
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0004] Conventional mechanical treatment methods have the following disadvantages: huge energy consumption
According to research reports, the power consumption of producing one ton of NFC products ranges from about 10,000 to hundreds of thousands of kilowatt-hours; the production cycle is relatively long, requiring multiple cycles and repeated processing; residual fibers affect the uniformity of product size
Chemical oxidation combined with mechanical treatment can significantly reduce energy consumption, but the current TEMPO chemical treatment method has high requirements on the purity of raw materials; TEMPO reagent consumes a lot, cannot be recycled, and the cost is high; when performing oxidation, sodium hypochlorite is required The solution is used as an oxidant, and sodium bromide or potassium bromide is added as an oxidation reaction aid
If the wastewater containing chlorine or bromine is discharged directly after production, it will seriously pollute the environment
Requires subsequent complex and costly water treatment
These problems limit the large-scale application of TEMPO chemical oxidation in production.

Method used

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  • Method for producing NFC (nano-fibrillated cellulose)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A method for producing cellulose nanofilament, the specific steps are as follows:

[0034] (1) 200 grams of poplar dissolving pulp boards were pre-soaked with 5 times the weight of distilled water for 60 minutes at room temperature (25° C.), and fully disintegrated. Adjust the slurry concentration to 15% (w / w) and use a medium-concentration hydraulic disc refiner for pretreatment. The pulp freeness was reduced to 130.

[0035] (2) Use NaAC-HAC buffer (pH=5.0) with a concentration of 0.1M to adjust the slurry concentration to 5% (w / w). The amount of cellulase added is 2.0×10 4 FPU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 50° C. for 30 minutes.

[0036] (3) Acidic oxidation solution is prepared by mixing 70% (w / w) hydrogen peroxide solution and 72% (w / w) sulfuric acid solution at 15°C, the molar ratio is 1:1.9, and the reaction time is 50 minutes. The stabilizer MgSO was added dropwise to the reaction solution 4 The...

Embodiment 2

[0040] A method for producing cellulose nanofilament, the specific steps are as follows:

[0041] (1) 300 grams of spruce organic solvent pulp, with a freeness of 100 after disc refining.

[0042] (2) The use concentration is 0.2MK 2 HPO 4 -KH 2 PO 4 Buffer (pH=7.0) was used to adjust the slurry concentration to 10% (w / w). The amount of xylanase added was 4.0×10 5 IU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 70° C. for 60 minutes.

[0043] (3) Alkaline oxidation solution is prepared by mixing 50% (w / w) hydrogen peroxide solution and 98% (w / w) sulfuric acid solution at 15°C, the molar ratio is 1:1.6, and the reaction time is 60 minutes. 1M K was added dropwise to the reaction solution 2 CO 3 The solution, the dropwise amount is alkaline reagent: sulfuric acid molar ratio is 1:1.5. Then add SDS at a final concentration of 0.1M as a diffusing agent. The yield of potassium persulfate was 50% of theory.

[0044] (3) The ...

Embodiment 3

[0047] (1) 300 grams of moso bamboo chemical pulp, with a freeness of 150 after refining with a disc refiner.

[0048] (2) Use K with a concentration of 0.2M 2 HPO 4 -KH 2 PO 4 Buffer (pH=7.0) was used to adjust the slurry concentration to 10% (w / w). The amount of mannanase added was 3.5×10 5 IU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 60° C. for 90 minutes.

[0049] (3) Alkaline oxidation solution is prepared by mixing 50% (w / w) hydrogen peroxide solution and 98% (w / w) sulfuric acid solution at 15°C, the molar ratio is 1:1.6, and the reaction time is 60 minutes. 1M K was added dropwise to the reaction solution 2 CO 3 The solution, the dropwise amount is alkaline reagent: sulfuric acid molar ratio is 1:1.5. The yield of potassium persulfate was 50% of theory.

[0050] (4) The pulp suspension pretreated by cellulase is filtered and washed twice with water, and the pulp concentration is adjusted to 8% (w / w). Potassium...

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Abstract

The invention discloses a method for producing NFC (nano-fibrillated cellulose). The method comprises the following steps that cellulose raw materials subjected to mechanical slurry grinding processing is diluted by a buffer solution; hemicellulase and / or cellulose are / is added for enzyme pretreatment; then, a mixture formed by peroxoic acid and one or more than two kinds of metal salts of the peroxoic acid is used as oxidization liquid for oxidizing fiber subjected to enzyme pretreatment; next, the oxidized cellulose is subjected to mechanical emulsification, and the NFC is obtained. The method is simple and efficient; the energy consumption and the pollution discharge in the production process can also be greatly reduced. When the technology is used for producing the NFC; the production period is obviously shortened; the mechanical energy consumption is greatly reduced; the production cost is low; the efficiency is high; the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the fields of green chemistry, biomass energy and materials, and specifically relates to the production and preparation of renewable functional biological materials using green chemistry methods. Background technique [0002] Cellulose is an important natural structural component of plant tissue, supporting and protecting it. The fibers in wood are usually filamentous, with a width of 5-10 microns and a length of 10-30 microns. It has the advantages of wide distribution, huge reserves and renewable. At the same time, wood cellulose is also an important raw material for the production of biomass fuel and biomass refining, and is widely used in pulp and paper, textile and hydrolysis to produce fermented sugar and other fields. The basic structural unit of cellulose is a linear glucose chain formed by the connection of glucose through glycosidic bonds. Multiple glucose chains are stacked together to form fibrils. The fiber pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02D21C9/00
Inventor 田霄飞刘明友卢娴肖仙英
Owner SOUTH CHINA UNIV OF TECH
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