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Preparation method of carboxylated cellulose nanoparticles

A technology of carboxylated cellulose and nanoparticles, which is applied in the field of cellulose, can solve the problems of complex and time-consuming preparation process, insufficient operation, toxicity, etc., and achieve the effects of simple and easy operation, environmental protection in the preparation process, and poor dispersion

Inactive Publication Date: 2016-08-24
DONGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the methods for preparing carboxylated cellulose nanomaterials mainly include: adopting ammonium persulfate oxidation system, the carboxylation degree is higher, but the required processing time is longer (CN 102911273 B); using hydrogen peroxide oxidation system, the preparation process is complicated Time-consuming, and the degree of carboxylation of cellulose is not high (CN 104017090 A); using NaClO in ionic liquid 4 +K 2 FeO 4 Oxidation system, the reaction conditions are relatively harsh, and the price of ionic liquid is high, and the economic benefit is low (CN105131130 A)
The most commonly used TEMPO (2,2,6,6,-tetramethylpiperidine oxynitride radical) oxidation system (CN 103157515B, CN 103570967 A, CN 105175557 A, CN 105315480 A) has a high degree of carboxylation, but The operation is not easy enough, TEMPO is expensive and has certain toxicity
[0005] The use of mixed acid treatment is expected to convert the hydroxyl groups on the surface of cellulose nanoparticles into other functional groups while preparing cellulose nanoparticles, such as hydrochloric acid and formic acid (CN 104153120 A) or citric acid and nitric acid, sulfuric acid, hydrochloric acid, etc. (CN104018235 A) Aldehydated cellulose nanoparticles are prepared by mixing, but the preparation process takes a long time, the yield is not high, and post-treatments such as alkali neutralization and centrifugation are required

Method used

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  • Preparation method of carboxylated cellulose nanoparticles
  • Preparation method of carboxylated cellulose nanoparticles
  • Preparation method of carboxylated cellulose nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Fully infiltrate commercially available microcrystalline cellulose in a mixed solution of 5 mol / L aqueous hydrochloric acid and 3 mol / L aqueous nitric acid, where the volume ratio of hydrochloric acid to nitric acid is 3:1, and then transfer it to a hydrothermic tank with a polytetrafluoroethylene liner. In the kettle; wherein, the solid content of microcrystalline cellulose in the mixed solution is 0.04g / mL. The reaction was carried out at 120° C. for 3 h. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. The solution is washed to be close to neutral by suction filtration to obtain a uniformly distributed dispersion of carboxylated cellulose nanoparticles; freeze-dried to obtain carboxylated cellulose nanoparticles. like figure 1 Scanning electron microscope observation shows that the prepared cellulose nanoparticles are rod-shaped, with a length of 100-300nm and a diameter of 5-20nm. figure 2 ...

Embodiment 2

[0038] Fully soak the manufactured paper in a mixed solution of 2mol / L hydrochloric acid aqueous solution and 1mol / L perchloric acid aqueous solution, wherein the volume ratio of hydrochloric acid to perchloric acid is 1:1, and then transfer it to a hydrothermal kettle lined with polytetrafluoroethylene Medium; Among them, the solid content of the paper in the mixed solution is 0.02g / mL. The reaction was carried out at 80° C. for 6 h. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. The solution is washed to be close to neutral by suction filtration to obtain a uniformly distributed dispersion of carboxylated cellulose nanoparticles; freeze-dried to obtain carboxylated cellulose nanoparticles. like image 3 Scanning electron microscope observation shows that the prepared cellulose nanoparticles are rod-shaped, with a length of 140-310nm and a diameter of 6-25nm. Figure 4 The carboxyl peak appeared in t...

Embodiment 3

[0040] The wood pulp is fully soaked in the mixed solution of 1mol / L hydrochloric acid aqueous solution and 5mol / L hypochlorous acid aqueous solution, wherein the volume ratio of hydrochloric acid and hypochlorous acid is 2:3, and then transferred to a hydrothermal kettle lined with polytetrafluoroethylene Medium; wherein, the solid content of wood pulp in the mixed solution is 0.01g / mL. The reaction was carried out at 100° C. for 0.5 h. After the hydrothermal kettle was naturally cooled, the reaction product was poured out and diluted with deionized water. The solution is washed to be close to neutral by suction filtration to obtain a uniformly distributed dispersion of carboxylated cellulose nanoparticles; freeze-dried to obtain carboxylated cellulose nanoparticles. like Figure 5 Scanning electron microscope observation shows that the prepared cellulose nanoparticles are rod-shaped, with a length of 120-310nm and a diameter of 8-22nm. Image 6 The carboxyl peak appeared i...

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Abstract

The invention relates to a preparation method of carboxylated cellulose nanoparticles. The preparation method comprises the following steps of soaking a cellulose raw material in a reaction liquid; carrying out hydrothermal reaction for 0.5-6 hours at the temperature of 80-120 DEG C; diluting a reaction product with water; carrying out suction filtration and washing repeatedly until washing liquor is neutral; and carrying out freeze drying to obtain the carboxylated cellulose nanoparticles, wherein the reaction liquid is mixed liquid of an oxidizing substance aqueous solution and a hydrochloric acid aqueous solution, and oxidizing substances are at least one of oxidizing acid and oxidizing salt. The method is simple and convenient in technology, easy to operate, low in cost and short in treatment time; the product is not required to be subjected to troublesome aftertreatment such as dialysis, and the prepared cellulose nanoparticles are high in purity, narrow in size distribution and easy to regulate and control; and the carboxylated cellulose nanoparticles are suitable for industrial large-scale production, and have wide application prospect in the fields of green nano composite materials, biological medicines, food, garments, cosmetics, coating, photoelectricity and the like.

Description

technical field [0001] The invention belongs to the technical field of cellulose, in particular to a preparation method of carboxylated cellulose nanoparticles. Background technique [0002] With the increasing scarcity of non-renewable resources and the increasing environmental pollution, the development and utilization of biodegradable materials have been paid more and more attention. As a natural biodegradable polymer material with the most abundant reserves, the widest distribution and the largest content in the world, cellulose has been widely used in the fields of textiles, construction engineering, papermaking and food. In recent years, cellulose-derived materials extracted from cellulose-cellulose nanoparticles are a new type of biomass-based nanomaterials, which have the characteristics of light weight, biodegradability, biocompatibility and regeneration of biological materials. In particular, cellulose nanocrystals also have high purity, high crystallinity, high Y...

Claims

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Application Information

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IPC IPC(8): C08B15/04B82Y40/00
CPCB82Y40/00C08B15/04
Inventor 秦宗益程淼任子初胡铄曾凡鑫陈园余刘嘉明
Owner DONGHUA UNIV
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