CN107286362A - A kind of preparation method of antibacterial NCC films - Google Patents
A kind of preparation method of antibacterial NCC films Download PDFInfo
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- CN107286362A CN107286362A CN201710532224.0A CN201710532224A CN107286362A CN 107286362 A CN107286362 A CN 107286362A CN 201710532224 A CN201710532224 A CN 201710532224A CN 107286362 A CN107286362 A CN 107286362A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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Abstract
The invention discloses a kind of preparation method of antibacterial NCC films, comprise the following steps：(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasound, stands, obtain NCC dispersion liquids；(2) the NCC dispersion liquids in step (1) are produced into NCC films with filtration method, obtains the electronegative NCC films in surface；(3) 50 200mL/m are pressed to the electronegative NCC films in obtained surface in step (2) with silver nitrate aqueous solution2Specification carries out 1 10 spray process, and is dried every time after spray, obtains surface deposition Ag+NCC films.The present invention proposes a kind of surface deposition Ag+New antibacterial NCC film preparation method, this method is simple and easy to apply, and cost is low, and NCC film dimensions and anti-microbial property can all realize regulation and control, and NCC wide material sources, therefore with good practicality.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of preparation method of antibacterial NCC films.
Background technology
Nano-cellulose (NCC) is diameter ＜ 100nm, and length can arrive the fiber aggregate of micron.It has excellent machine
Tool performance, huge specific surface area, high-crystallinity, high-hydrophilic, the high grade of transparency, low-density, good biodegradability, life
Thing compatibility and stable chemical property.Therefore, nano-cellulose bio-pharmaceuticals, food processing, papermaking, energy and material,
The fields such as functional material have shown that huge application potential.
NCC films have excellent mechanical performance, optical property and the barrier different from general fibre film, and this is tied with it
Structure has the relation of interwoveness.Macroscopically, NCC films are similar with common plastics.But can be observed under ESEM
Arrive, on the membrane surface, nano-cellulose is in disorderly arranged, and with nanoaperture structure, the size in hole generally 10 ~
Between 50nm, fiber is accumulated in stratiform in the vertical.What the porous three-dimensional layer structure of NCC films can alleviate that paper bears should
Power, so as to assign film excellent mechanical property.But tradition NCC films do not have antibacterial action.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art there is provided a kind of preparation of antibacterial NCC films
Method,.
A kind of preparation method of antibacterial NCC films, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasound, stands, obtain NCC dispersion liquids；
(2) the NCC dispersion liquids in step (1) are produced into NCC films with filtration method, obtains the electronegative NCC films in surface；
(3) take silver nitrate to be dissolved in distilled water and silver nitrate aqueous solution is made, with silver nitrate aqueous solution to obtained table in step (2)
The electronegative NCC films in face press 50-200mL/m2Specification carries out 1-10 spray process, and is dried every time after spray, obtains table
Face deposits Ag+NCC films.
Further, step（1）Described sonication treatment time is 10-100min.
Further, step（1）The concentration of described NCC dispersion liquids is 0.01%-0.2%.
Further, the silver nitrate solution concentration described in step (3) is 0.5% ~ 1%..
Further, the electronegative NCC in surface described in step (1) is made by sulphuric acid hydrolysis NCC raw material.
Preferably, the electronegative NCC in the described surface raw material that prepare are selected from cotton linter, waste paper or timber.
Further, the filtration method described in step (2) is：NCC dispersion liquids described in step (1) are removed by filter membrane
80% moisture, is made NCC gels, and NCC gels then are transferred into mould, applies 15N pressure, table is dried at normal temperatures
The electronegative NCC films in face.
Further, the filter membrane thickness is 0.45 μm.
Beneficial effects of the present invention：Method directly sprays silver nitrate aqueous solution in electronegative NCC film surfaces, by quiet
Electro ultrafiltration deposits Ag in NCC film surfaces+, it is proposed that a kind of surface deposits Ag+New antibacterial NCC film preparation method.
This method is simple and easy to apply, and cost is low, and NCC film dimensions and anti-microbial property can all realize regulation and control, and NCC wide material sources, therefore
With good practicality.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated,
Embodiment 1
A kind of preparation method of antibacterial NCC films, comprises the following steps：
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 10min, standing, obtain the NCC dispersion liquids that concentration is 0.01%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.5% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 50mL/m in2Specification carries out 1 spray process, then dries, obtains surface
Deposit Ag+NCC films.
Embodiment 2
A kind of preparation method of antibacterial NCC films, comprises the following steps：
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 100min, standing, obtain the NCC dispersion liquids that concentration is 0.2%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 1% is made, with silver nitrate aqueous solution to step (2)
In the obtained electronegative NCC films in surface press 200mL/m2Specification carries out spray process, then dries, the above-mentioned spray of repetition,
Drying process 10 times, obtains surface deposition Ag+NCC films.
Embodiment 3
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 55min, standing, obtain the NCC dispersion liquids that concentration is 0.1%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.8% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 125mL/m in2Specification carries out spray process, then dries, and repeats above-mentioned spray
Pouring, drying process 5 times, obtain surface deposition Ag+NCC films.
Embodiment 4
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 55min, standing, obtain the NCC dispersion liquids that concentration is 0.01%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 1% is made, with silver nitrate aqueous solution to step (2)
In the obtained electronegative NCC films in surface press 125mL/m2Specification carries out spray process, then dries, the above-mentioned spray of repetition,
Drying process 5 times, obtains surface deposition Ag+NCC films.
Embodiment 5
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 100min, standing, obtain the NCC dispersion liquids that concentration is 0.2%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.5% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 125mL/m in2Specification carries out spray process, then dries, and repeats above-mentioned spray
Pouring, drying process 10 times, obtain surface deposition Ag+NCC films.
Embodiment 6
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 10min, standing, obtain the NCC dispersion liquids that concentration is 0.1%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 1% is made, with silver nitrate aqueous solution to step (2)
In the obtained electronegative NCC films in surface press 50mL/m2Specification carries out spray process, then dries, and repeats above-mentioned spray, does
Dry process 5 times, obtains surface deposition Ag+NCC films.
Embodiment 7
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 100min, standing, obtain the NCC dispersion liquids that concentration is 0.1%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.5% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 200mL/m in2Specification carries out spray process, then dries, and repeats above-mentioned spray
Pouring, drying process 1 time, obtain surface deposition Ag+NCC films.
Embodiment 8
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 55min, standing, obtain the NCC dispersion liquids that concentration is 0.01%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.8% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 125mL/m in2Specification carries out spray process, then dries, and repeats above-mentioned spray
Pouring, drying process 6 times, obtain surface deposition Ag+NCC films.
Embodiment 9
(1) sulphuric acid hydrolysis cotton linter is obtained into the electronegative NCC in surface, the electronegative NCC in surface is scattered in deionized water
In, through ultrasonic 55min, standing, obtain the NCC dispersion liquids that concentration is 0.2%；
(2) the NCC dispersion liquids described in step (1) are removed by 0.45 μm of filter membrane 80% moisture, NCC gels are made, then
NCC gels are transferred to mould, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures；
(3) take silver nitrate to be dissolved in distilled water and the silver nitrate aqueous solution that concentration is 0.7% is made, with silver nitrate aqueous solution to step
(2) the electronegative NCC films in obtained surface press 125mL/m in2Specification carries out spray process, then dries, and repeats above-mentioned spray
Pouring, drying process 6 times, obtain surface deposition Ag+NCC films.
Surface made from above-described embodiment 1-9 is deposited into Ag+NCC films, anti-microbial property test, test side are carried out respectively
Method is：Using LB culture mediums, 10uL standard E. colis, staphylococcus aureus and the addition of bacillus subtilis bacteria suspension are respectively taken
Activated into the sterile LB liquid mediums of 5mL, the bacteria suspension of activation is diluted to 10-5cfu/mL.0.1 mL bacteriums are taken to hang
Liquid is uniformly sprayed at 50mm × 50mm NCC film surfaces, and 20h is cultivated in 37 DEG C of incubators, observes surface colony situation.Will
Test result statistics such as following table：
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Test result | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found | Bacterium colony is not found |
The test result shown in upper table, NCC films have good anti-microbial property made from method of the invention.
In a word, the present invention proposes a kind of surface deposition Ag+New antibacterial NCC film preparation method, this method
Simple and easy to apply, cost is low, and NCC film dimensions and anti-microbial property can all realize regulation and control, and NCC wide material sources, therefore with very
Good practicality.
Claims (8)
1. a kind of preparation method of antibacterial NCC films, it is characterised in that comprise the following steps：
(1) the electronegative NCC in surface is scattered in deionized water, through ultrasound, stands, obtain NCC dispersion liquids；
(2) the NCC dispersion liquids in step (1) are produced into NCC films with filtration method, obtains the electronegative NCC films in surface；
(3) take silver nitrate to be dissolved in distilled water and silver nitrate aqueous solution is made, with silver nitrate aqueous solution to obtained table in step (2)
The electronegative NCC films in face press 50-200mL/m2Specification carries out 1-10 spray process, and is dried every time after spray, obtains table
Face deposits Ag+NCC films.
2. the preparation method of antibacterial NCC films according to claim 1, it is characterised in that step（1）Described ultrasound
Processing time is 10-100min.
3. the preparation method of antibacterial NCC films according to claim 1, it is characterised in that step（1）Described NCC points
The concentration of dispersion liquid is 0.01%-0.2%.
4. the preparation method of antibacterial NCC films according to claim 1, it is characterised in that the nitric acid described in step (3)
Silver-colored solution concentration is 0.5% ~ 1%.
5. the preparation method of antibacterial NCC films according to claim 1, it is characterised in that the surface band described in step (1)
The NCC of negative electricity is made by sulphuric acid hydrolysis NCC raw material.
6. the preparation method of antibacterial NCC films according to claim 1 or 5, it is characterised in that described surface is negatively charged
NCC prepare raw material be selected from cotton linter, waste paper or timber.
7. the preparation method of antibacterial NCC films according to claim 1, it is characterised in that the filtration method described in step (2)
For：NCC dispersion liquids described in step (1) are removed by filter membrane 80% moisture, NCC gels are made, then turn NCC gels
Mould is moved on to, applies 15N pressure, the electronegative NCC films in surface is dried at normal temperatures.
8. the preparation method of antibacterial NCC films according to claim 7, it is characterised in that the filter membrane thickness is 0.45 μ
m。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776869A (en) * | 2018-12-29 | 2019-05-21 | 华南理工大学 | A kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, preparation method and application |
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| WO2013132491A2 (en) * | 2012-03-06 | 2013-09-12 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Light spectrum tunable nanocomposites |
| CN103467766A (en) * | 2013-09-15 | 2013-12-25 | 浙江理工大学 | Rapid preparation method of totally-biodegradable composite membrane with nanometer silver on surface |
| CN105053007A (en) * | 2015-08-06 | 2015-11-18 | 北京科技大学 | Preparation method of novel high performance antibacterial nano-cellulose carbon aerogel |
| CN105778138A (en) * | 2014-12-13 | 2016-07-20 | 广东轻工职业技术学院 | Nano-silver composite antibacterial cellulose membrane, and preparation method and application thereof |
-
2017
- 2017-07-03 CN CN201710532224.0A patent/CN107286362B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013132491A2 (en) * | 2012-03-06 | 2013-09-12 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Light spectrum tunable nanocomposites |
| CN103467766A (en) * | 2013-09-15 | 2013-12-25 | 浙江理工大学 | Rapid preparation method of totally-biodegradable composite membrane with nanometer silver on surface |
| CN105778138A (en) * | 2014-12-13 | 2016-07-20 | 广东轻工职业技术学院 | Nano-silver composite antibacterial cellulose membrane, and preparation method and application thereof |
| CN105053007A (en) * | 2015-08-06 | 2015-11-18 | 北京科技大学 | Preparation method of novel high performance antibacterial nano-cellulose carbon aerogel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776869A (en) * | 2018-12-29 | 2019-05-21 | 华南理工大学 | A kind of cellulose fixed nano silver of oxidation nanometer/grape seed extract antibacterial, anti-oxidant composite membrane, preparation method and application |
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