CN107383401A - A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group - Google Patents
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group Download PDFInfo
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- CN107383401A CN107383401A CN201710531983.5A CN201710531983A CN107383401A CN 107383401 A CN107383401 A CN 107383401A CN 201710531983 A CN201710531983 A CN 201710531983A CN 107383401 A CN107383401 A CN 107383401A
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- ncc
- sulfa drugs
- antibacterial
- scion grafting
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/43—Compounds containing sulfur bound to nitrogen
- C08K5/435—Sulfonamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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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 the antibacterial NCC films of surface scion grafting sulfa drugs group, comprise the following steps：(1) the electronegative nano-cellulose in surface is scattered in deionized water, obtains NCC dispersion liquids；(2) pH value that NCC dispersion liquids are adjusted with NaOH solution is 7.5 9.0；(3) sulfa drugs solution is added into resulting solution, is rapidly heated to 80 ~ 95 DEG C, cooling discharge after ultrasonic agitation reaction；(4) by step（3）Obtained reaction mixture prepares the antibacterial NCC films of surface scion grafting sulfa drugs group using filtration method.The present invention utilizes the amino group of sulfa drugs and NCC hydroxy combining, NCC film of the acquisition with anti-microbial property, and the addition of sulfanilamide (SN) simultaneously, to relax condition of storage in the antibiotic property for improving NCC films, improve the scope of application of NCC films.Cost of material is cheap simultaneously, and source is wide, suitable for generally producing popularization.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of antibacterial of surface scion grafting sulfa drugs group
The preparation method of 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 it can be observed under ESEM
Arrive, on the membrane surface, nano-cellulose has nanoaperture structure in disorderly arranged, 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 traditional NCC films do not have antibacterial action.
Sulfa drugs is a kind of broad spectrum antibiotic, be clinically mainly used in prevent and treat infectious diseases, in addition its
Property is stable, and manufacture is not required to grain and does the advantages that raw material, yield are big, wide in variety, price is low, easy to use, in liberal supply.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of surface scion grafting sulfa drugs
The preparation method of the antibacterial NCC films of group, this method is simple and easy, cheap, and NCC film dimensions are controllable, assign simultaneously
NCC film anti-microbial properties..
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasound, stands, obtain NCC dispersion liquids；
(2) with concentration be 20%-30% NaOH solution regulating step (1) obtained by NCC dispersion liquids pH value, make the pH value be
7.5-9.0；
(3) to step（2）Sulfa drugs solution is added in resulting solution, is rapidly heated to 80 ~ 95 DEG C, ultrasonic agitation reaction
It is cooled to 35-50 DEG C of discharging after 40-60min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 models in 2-4 DEG C/min
Enclose；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
Further, step（1）Described sonication treatment time is 10-100min, and the concentration of described NCC dispersion liquids is
0.01%-0.2%。
Further, the concentration of the NaOH solution described in step (2) is 25%.
Further, the temperature-rise period speed control described in step (3) is in 3 DEG C/min.
Further, the sulfa drugs solution described in step (3), is the sulfa drugs aqueous solution, concentration 0.8-
1.2g/L。
Further, the sulfa drugs be sulfadimidine, bacteresulf, sulphadiazine, sulfamethoxazole,
At least one of sulfametoxydiazine, sulfadimethoxine, phthalylsulfathiazol.
Further, the preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter, waste paper or wood
Material.
Beneficial effects of the present invention：(1) using the amino group of sulfa drugs and NCC hydroxy combining, without surface
It is modified, the NCC films of surface scion grafting sulfa drugs have been prepared, have realized the good anti-microbial property of NCC films；(2) and
NCC is easily destroyed, it is necessary to preserve at low temperature by bacterial corrosion in itself, and the addition of sulfanilamide (SN) is same in the antibiotic property for improving NCC films
When, improve the scope of application of NCC films；（3）Sulfa drugs is cheap, and source is wide, so surface scion grafting sulfonamides
The NCC films of thing have good price advantage；（4）The NCC method for manufacturing thin film of the present invention can be by controlling the size of filter membrane
The size of film is controlled, the thickness of film is controlled by filtration time, size is controllable, and according to use range, may be selected suitably
Sulfa drugs carries out scion grafting, so as to realize targetedly anti-microbial property.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated,
Embodiment 1
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 10nin, standing, obtaining concentration is
0.01% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 20% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulfadimidine aqueous solution that concentration is 0.8g/L is added in resulting solution, is rapidly heated to 80
DEG C, it is cooled to 35 DEG C of dischargings after ultrasonic agitation reaction 40min, temperature-rise period speed control is maintained at pH value in 2 DEG C/min
7.5-9.0 scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter.
Embodiment 2
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 100min, standing, obtaining concentration is
0.2% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 30% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The 1.2g/L bacteresulf aqueous solution is added in resulting solution, is rapidly heated to 95 DEG C, ultrasound is stirred
50 DEG C of dischargings are cooled to after mixing reaction 60min, and temperature-rise period speed control makes pH value be maintained at 7.5-9.0 models in 4 DEG C/min
Enclose；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter.
Embodiment 3
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 50min, standing, obtaining concentration is
0.1% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 25% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulfadimidine aqueous solution that concentration is 1.0g/L is added in resulting solution, is rapidly heated to 90
DEG C, it is cooled to 40 DEG C of dischargings after ultrasonic agitation reaction 50min, temperature-rise period speed control is maintained at pH value in 3 DEG C/min
7.5-9.0 scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter.
Embodiment 4
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 10min, standing, obtaining concentration is
0.2% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 20% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）It is the 0.8g/L sulfadimidine aqueous solution that concentration is added in resulting solution, is rapidly heated to 80 DEG C,
50 DEG C of dischargings are cooled to after ultrasonic agitation reaction 60min, and temperature-rise period speed control makes pH value be maintained at 7.5- in 3 DEG C/min
9.0 scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from timber.
Embodiment 5
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 100min, standing, obtaining concentration is
0.01% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 30% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulphadiazine aqueous solution that concentration is 1.2g/L is added in resulting solution, is rapidly heated to 95 DEG C, is surpassed
It is cooled to 35 DEG C of dischargings after sound stirring reaction 40min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 in 2 DEG C/min
Scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter, waste paper or timber.
Embodiment 6
A kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, comprises the following steps：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 100min, standing, obtaining concentration is
0.1% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 25% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulphadiazine aqueous solution that concentration is 1.2g/L is added in resulting solution, is rapidly heated to 90 DEG C, is surpassed
It is cooled to 40 DEG C of dischargings after sound stirring reaction 50min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 in 3 DEG C/min
Scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from timber.
Embodiment 7
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 60min, standing, obtaining concentration is
0.1% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 25% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulphadiazine aqueous solution that concentration is 0.8g/L is added in resulting solution, is rapidly heated to 90 DEG C, is surpassed
It is cooled to 40 DEG C of dischargings after sound stirring reaction 50min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 in 3 DEG C/min
Scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from timber.
Embodiment 8
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 60min, standing, obtaining concentration is
0.2% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 25% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulphadiazine aqueous solution that concentration is 1.0g/L is added in resulting solution, is rapidly heated to 90 DEG C, is surpassed
It is cooled to 40 DEG C of dischargings after sound stirring reaction 50min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 in 3 DEG C/min
Scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from timber.
Embodiment 9
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasonic 60min, standing, obtaining concentration is
0.01% NCC dispersion liquids；
(2) pH value of the NCC dispersion liquids obtained by the NaOH solution regulating step (1) for being 25% with concentration, it is 7.5- to make pH value
9.0；
(3) to step（2）The sulphadiazine aqueous solution that concentration is 1.0g/L is added in resulting solution, is rapidly heated to 90 DEG C, is surpassed
It is cooled to 40 DEG C of dischargings after sound stirring reaction 50min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 in 3 DEG C/min
Scope；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
The preparing raw material of the electronegative nano-cellulose in described surface is selected from timber.
In a word, the present invention is modified without surface, obtained using the amino group of sulfa drugs and NCC hydroxy combining
NCC films with anti-microbial property, and the addition of sulfanilamide (SN) improve NCC films antibiotic property simultaneously, relax condition of storage,
Improve the scope of application of NCC films.Cost of material is cheap simultaneously, and source is wide, suitable for generally producing popularization.
Claims (7)
1. a kind of preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group, it is characterised in that including following step
Suddenly：
(1) the electronegative nano-cellulose in surface is scattered in deionized water, through ultrasound, stands, obtain NCC dispersion liquids；
(2) with concentration be 20%-30% NaOH solution regulating step (1) obtained by NCC dispersion liquids pH value, make the pH value be
7.5-9.0；
(3) to step（2）Sulfa drugs solution is added in resulting solution, is rapidly heated to 80-95 DEG C, ultrasonic agitation reaction
It is cooled to 35-50 DEG C of discharging after 40-60min, temperature-rise period speed control makes pH value be maintained at 7.5-9.0 models in 2-4 DEG C/min
Enclose；
(4) by step（3）Obtained reaction mixture prepares film using filtration method, obtains surface scion grafting sulfa drugs group
Antibacterial NCC films.
2. the preparation method of the antibacterial NCC films of scion grafting sulfa drugs group in surface according to claim 1, its feature
It is, step（1）Described sonication treatment time is 10-100min, and the concentration of described NCC dispersion liquids is 0.01%-0.2%.
3. the preparation method of the antibacterial NCC films of scion grafting sulfa drugs group in surface according to claim 1, its feature
It is, the concentration of the NaOH solution described in step (2) is 25%.
4. the preparation method of the antibacterial NCC films of scion grafting sulfa drugs group in surface according to claim 1, its feature
It is, the temperature-rise period speed control described in step (3) is in 3 DEG C/min.
5. the preparation method of the antibacterial NCC films of scion grafting sulfa drugs group in surface according to claim 1, its feature
It is, the sulfa drugs solution described in step (3), is the sulfa drugs aqueous solution, concentration 0.8-1.2g/L.
6. the preparation method of the antibacterial NCC films of surface scion grafting sulfa drugs group according to claim 1 or 5, its
It is characterised by, the sulfa drugs is sulfadimidine, bacteresulf, sulphadiazine, sulfamethoxazole, kynix
At least one of pyrimidine, sulfadimethoxine, phthalylsulfathiazol.
7. the preparation method of the antibacterial NCC films of scion grafting sulfa drugs group in surface according to claim 1, its feature
It is, the preparing raw material of the electronegative nano-cellulose in described surface is selected from cotton linter, waste paper or timber.
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| CN201710531983.5A CN107383401B (en) | 2017-07-03 | 2017-07-03 | Preparation method of antibacterial NCC film with surface grafted with sulfonamide group |
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| CN201710531983.5A CN107383401B (en) | 2017-07-03 | 2017-07-03 | Preparation method of antibacterial NCC film with surface grafted with sulfonamide group |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905031A (en) * | 2010-07-16 | 2010-12-08 | 北京科技大学 | Method for preparing flamazine/bacterial cellulose composite wound dressing |
| US20150240411A1 (en) * | 2012-08-14 | 2015-08-27 | Technicka Univerzita V Liberci | Nanofiber structure with immobilized organic substance and the method of its preparation |
| CN104874015A (en) * | 2015-06-05 | 2015-09-02 | 四川大学 | Bacterial-cellulose dressing with antibacterial and bacteriostatic functions and preparation method as well as application thereof |
-
2017
- 2017-07-03 CN CN201710531983.5A patent/CN107383401B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905031A (en) * | 2010-07-16 | 2010-12-08 | 北京科技大学 | Method for preparing flamazine/bacterial cellulose composite wound dressing |
| US20150240411A1 (en) * | 2012-08-14 | 2015-08-27 | Technicka Univerzita V Liberci | Nanofiber structure with immobilized organic substance and the method of its preparation |
| CN104874015A (en) * | 2015-06-05 | 2015-09-02 | 四川大学 | Bacterial-cellulose dressing with antibacterial and bacteriostatic functions and preparation method as well as application thereof |
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