CN107286362B - Preparation method of antibacterial NCC film - Google Patents

Preparation method of antibacterial NCC film Download PDF

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Publication number
CN107286362B
CN107286362B CN201710532224.0A CN201710532224A CN107286362B CN 107286362 B CN107286362 B CN 107286362B CN 201710532224 A CN201710532224 A CN 201710532224A CN 107286362 B CN107286362 B CN 107286362B
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ncc
film
silver nitrate
dispersion liquid
ncc film
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CN107286362A (en
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陈照峰
沈胜
张俊雄
胡雅
叶信立
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Suzhou Superlong Aviation Heat Resistance Material Technology Co Ltd
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Suzhou Superlong Aviation Heat Resistance Material Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C08J7/14—Chemical modification with acids, their salts or anhydrides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a preparation method of an antibacterial NCC film, which comprises the following steps: (1) dispersing the nano-cellulose with the negative electricity on the surface in deionized water, and performing ultrasonic treatment and standing to obtain NCC dispersion liquid; (2) filtering the NCC dispersion liquid in the step (1) to produce an NCC film to obtainTo a NCC film with a negative surface charge; (3) using silver nitrate aqueous solution to treat the NCC film with the negative surface prepared in the step (2) according to the volume ratio of 50-200mL/m2Spraying for 1-10 times, and drying after each spraying to obtain Ag deposited on the surface+The NCC film of (2). The invention provides a method for depositing Ag on the surface+The preparation method of the novel antibacterial NCC film is simple and easy to implement, low in cost, capable of realizing regulation and control of the size and the antibacterial performance of the NCC film, and wide in NCC source, so that the method has good practicability.

Description

Preparation method of antibacterial NCC film
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of an antibacterial NCC film.
Background
Nanocellulose (NCC) is a collection of fibres with a diameter < 100nm and a length of up to a micron. It has excellent mechanical performance, great specific surface area, high crystallinity, high hydrophilicity, high transparency, low density, excellent biodegradability, biocompatibility and stable chemical property. Therefore, nanocellulose has shown great application potential in the fields of biopharmaceuticals, food processing, papermaking, energy materials, functional materials and the like.
The NCC film has excellent mechanical property, optical property and barrier property which are different from those of common fiber films, and the NCC film has an inseparable relationship with the structure of the NCC film. On a macroscopic scale, NCC films are similar to ordinary plastics. However, under a scanning electron microscope, it can be observed that on the surface of the film, the nanocellulose is in disordered arrangement and has a nanometer pore structure, the size of pores is usually between 10 nm and 50nm, and the fibers are stacked in a layered manner in the longitudinal direction. The porous three-dimensional layered structure of the NCC film can relieve the stress borne by paper, so that the film is endowed with excellent mechanical properties. However, conventional NCC films do not have an antibacterial effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an antibacterial NCC film.
A preparation method of an antibacterial NCC film comprises the following steps:
(1) dispersing the nano-cellulose with the negative electricity on the surface in deionized water, and performing ultrasonic treatment and standing to obtain NCC dispersion liquid;
(2) producing an NCC film by using the NCC dispersion liquid in the step (1) through a filtration method to obtain an NCC film with a negative surface;
(3) dissolving silver nitrate in distilled water to obtain silver nitrate water solution, and treating the NCC film with negative electricity on the surface prepared in step (2) with the silver nitrate water solution according to the ratio of 50-200mL/m2Spraying for 1-10 times, and drying after each spraying to obtain Ag deposited on the surface+The NCC film of (2).
Further, the ultrasonic treatment time in the step (1) is 10-100 min.
Further, the concentration of the NCC dispersion liquid in the step (1) is 0.01-0.2%.
Further, the concentration of the silver nitrate solution in the step (3) is 0.5% -1%. .
Further, the NCC with negatively charged surface described in the step (1) is prepared by hydrolyzing NCC raw material with sulfuric acid.
Preferably, the raw material for the preparation of the NCC with negatively charged surface is selected from cotton linters, waste paper or wood.
Further, the filtration method in the step (2) is as follows: removing 80% of water from the NCC dispersion liquid in the step (1) through a filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain the NCC film with the negative surface.
Further, the filter membrane thickness is 0.45 μm.
The invention has the beneficial effects that: the method directly sprays silver nitrate aqueous solution on the surface of the NCC film with negative electricity, and deposits Ag on the surface of the NCC film through electrostatic action+A surface deposited Ag is proposed+A method for producing the novel film of antibacterial NCC. The method is simple and easy to implement, has low cost, can realize the regulation and control of the size and the antibacterial performance of the NCC film, and has wide NCC sources, thereby having good practicability.
Detailed Description
The invention will be further elucidated with reference to the embodiments described hereinafter,
example 1
A preparation method of an antibacterial NCC film comprises the following steps:
(1) hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 10min, and standing to obtain NCC dispersion liquid with concentration of 0.01%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.5% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 50mL/m2Spraying for 1 time according to the specification, and then drying to obtain the surface deposited Ag+The NCC film of (2).
Example 2
A preparation method of an antibacterial NCC film comprises the following steps:
(1) hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 100min, and standing to obtain NCC dispersion liquid with concentration of 0.2%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 1% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 200mL/m2Spraying, drying, and repeating the spraying and drying process for 10 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 3
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 55min, and standing to obtain NCC dispersion liquid with concentration of 0.1%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.8% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 125mL/m2Spraying, drying, and repeating the spraying and drying process for 5 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 4
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 55min, and standing to obtain NCC dispersion liquid with concentration of 0.01%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 1% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 125mL/m2Spraying, drying, and repeating the spraying and drying process for 5 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 5
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 100min, and standing to obtain NCC dispersion liquid with concentration of 0.2%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.5% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 125mL/m2Spraying, drying, and repeating the spraying and drying process for 10 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 6
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 10min, and standing to obtain NCC dispersion liquid with concentration of 0.1%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 1% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 50mL/m2Spraying, drying, and repeating the spraying and drying process for 5 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 7
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 100min, and standing to obtain NCC dispersion liquid with concentration of 0.1%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.5% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 200mL/m2Spraying according to the specification, drying, and repeating the spraying and drying processes for 1 time to obtain Ag deposited on the surface+The NCC film of (2).
Example 8
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 55min, and standing to obtain NCC dispersion liquid with concentration of 0.01%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.8% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 125mL/m2Spraying according to the specification, drying, and repeating the spraying and drying processes for 6 times to obtain Ag deposited on the surface+The NCC film of (2).
Example 9
(1) Hydrolyzing cotton linters with sulfuric acid to obtain NCC with negative surface, dispersing the NCC with negative surface in deionized water, performing ultrasonic treatment for 55min, and standing to obtain NCC dispersion liquid with concentration of 0.2%;
(2) removing 80% of water from the NCC dispersion liquid in the step (1) through a 0.45-micron filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negatively charged surface;
(3) dissolving silver nitrate in distilled water to obtain 0.7% silver nitrate aqueous solution, and treating the NCC film with negative surface charge prepared in step (2) with the silver nitrate aqueous solution at a ratio of 125mL/m2Spraying according to the specification, drying, and repeating the spraying and drying processes for 6 times to obtain Ag deposited on the surface+The NCC film of (2).
The surface-deposited Ag prepared in examples 1 to 9 was subjected to+The NCC film is respectively subjected to antibacterial performance test, and the test method comprises the following steps: using LB culture medium, respectively taking 10uL of standard Escherichia coli, staphylococcus aureus and Bacillus subtilis bacterial suspension, adding into 5mL of sterile LB liquid culture solution for activation, and diluting the activated bacterial suspension to 10-5cfu/mL. 0.1 mL of the bacterial suspension was uniformly sprayed on the surface of a NCC film of 50mm X50 mm, and the film was cultured in an incubator at 37 ℃ for 20 hours to observe the surface colony. The test results are statistically shown in the following table:
examples 1 2 3 4 5 6 7 8 9
Test results No colonies were found No colonies were found No colonies were found No colonies were found No colonies were found No colonies were found No colonies were found No colonies were found No colonies were found
As can be seen from the test results shown in the above table, the NCC film prepared by the method of the present invention has excellent antibacterial properties.
In summary, the present invention provides a method for depositing Ag on a surface+The preparation method of the novel film of antibacterial NCCThe method is simple and easy to implement, has low cost, can realize regulation and control of the size and the antibacterial performance of the NCC film, and has wide NCC sources, thereby having good practicability.

Claims (1)

1. A preparation method of an antibacterial NCC film is characterized by comprising the following steps:
(1) dispersing NCC with negative electricity on the surface in deionized water, carrying out ultrasonic treatment for 10-100min, and standing to obtain NCC dispersion liquid with the concentration of 0.01-0.2%; the NCC with the negative surface is prepared by hydrolyzing an NCC raw material by sulfuric acid; the raw material is selected from cotton linter, waste paper or wood;
(2) producing an NCC film by using the NCC dispersion liquid in the step (1) through a filtration method to obtain an NCC film with a negative surface; the filtration method comprises the following steps: removing 80% of water from the NCC dispersion liquid in the step (1) through a filter membrane to prepare NCC gel, transferring the NCC gel to a mould, applying a pressure of 15N, and drying at normal temperature to obtain an NCC film with a negative surface;
(3) dissolving silver nitrate in distilled water to prepare a silver nitrate water solution with the concentration of 0.5-1%, and carrying out 50-200mL/m treatment on the NCC film with the negative electricity on the surface prepared in the step (2) by using the silver nitrate water solution2Spraying for 1-10 times, and drying after each spraying to obtain Ag deposited on the surface+The NCC film of (2).
CN201710532224.0A 2017-07-03 2017-07-03 Preparation method of antibacterial NCC film Active CN107286362B (en)

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