Nanometer fibrils cellulose surface hydrophobic modification method

A technology of nanocellulose and hydrophobic modification, which is applied in the field of nanocellulose and achieves the effects of strong controllability, simple and easy preparation method and short reaction period.

Inactive Publication Date: 2018-07-10
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the hydrophobic modification of nano-cellulose by alkyl ketene dimer and alkenyl succinic anhydride, only the patent CN104499361B discloses a kind of AKD sizing agent containing nano-microcrystalline cellulose, preparation method and its purpose

Method used

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  • Nanometer fibrils cellulose surface hydrophobic modification method
  • Nanometer fibrils cellulose surface hydrophobic modification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Place 2000mL of toluene and 100g of freeze-dried unmodified nanofibril cellulose powder in a 5L reactor with a stirring and condensing reflux device, start the stirring device, mix the solvent and nanocellulose evenly, and adjust the temperature to 90°C. Take 5g, 10g, 20g, 30g, 50g of AKD wax powder and dissolve it with 100g of toluene. After the AKD wax powder is completely dissolved, add it to the reactor to start the grafting reaction, keep the temperature, and the reaction time is 6 hours . After the reaction is finished, the reactants are washed with toluene, the unreacted toluene solvent and the unreacted AKD are recovered, and the dry hydrophobic nanofibril cellulose fibers are obtained after filtering, volatilizing, and collecting the organic solvent. The properties of nanocellulose after the reaction are shown in Table 10.

[0044] AKD(g)

Embodiment 2

[0046]Put 2000mL of toluene and 100g of freeze-dried TEMPO oxidized nanocellulose powder in a 5L reactor with a stirring and condensing reflux device, start the stirring device, mix the solvent and nanocellulose evenly, and adjust the temperature to 120 ℃. Take 30g of AKD wax powder, dissolve it in 100g of toluene and add it into the reactor, keep the temperature, and the reaction time is 4 hours. After the reaction, use toluene to wash the reactant, recover the unreacted toluene solvent and unreacted AKD, filter and volatilize the organic solvent and then hydrophobic nano-fibril cellulose fibers, the modified nano-cellulose can be dispersed in Organic solvents such as isopropanol and methylene chloride.

Embodiment 3

[0048] Place 3000mL N, N-dimethylformamide and 300g freeze-dried TEMPO nanofibril cellulose powder in a 5L reactor with a stirring and condensing reflux device, start the stirring device, and mix the solvent with the nanofiber Mix the ingredients evenly, and adjust the temperature to 60°C. Weigh 4, add lutidine 15g to the reaction system and stir for 15 minutes, weigh dodecenyl succinic anhydride 15g, 30g, 50g, 100g, 150g and add to the system, keep the reaction temperature and stirring, the reaction time is 8 Hour. After the reaction, filter the reactant with suction to recover unreacted dodecenyl succinic anhydride and N,N-dimethylformamide, wash and dry to obtain nanofibrillar cellulose fibers modified by dodecenyl succinic anhydride . The performance of the nanocellulose after the reaction is as follows:

[0049]

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Abstract

The invention provides a nanometer fibrils cellulose surface hydrophobic modification method. Alkenyl succinic anhydride or alkyl ketene dimer is grafted onto nanometer cellulose surface; partial hydrophile groups such as hydroxyl and carboxyl are replaced, so that the goal of changing the surface energy of the nanometer fiber is achieved, so that the super-hydrophilicity performance is convertedinto hydrophobic performance; finally, the application field can be expanded. The process has the advantages that the process operation is simple; the cost is low; the effect is obvious.

Description

technical field [0001] The invention relates to the field of nanocellulose, and more specifically relates to a method of hydrophobizing and modifying the surface of nanocellulose by using a papermaking method reactive sizing agent. Background technique [0002] Nanocellulose includes nanofibrillated cellulose and nanocrystalline cellulose, which are filamentous cellulose fibers separated from plant cellulose with a diameter of 5-20 nm and a length of several hundred nanometers to tens of microns. As a new type of nanofiber material, nanocellulose not only has the characteristics of cellulose, but also has many characteristics of nanomaterials, such as huge specific surface area, high Young's modulus, super adsorption capacity and high reaction activity, which makes it very different from ordinary cellulose in properties, so it is favored by researchers at home and abroad. In recent years, there have been many researches on the application of nanocellulose gels and fibers, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/02C08F222/04C08F220/10
CPCC08F251/02C08F222/04C08F220/10
Inventor 温洋兵曲家磊刘雄利
Owner TIANJIN UNIV OF SCI & TECH
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