CN110373735A - A kind of preparation method based on polyelectrolyte surfactant complexes antibacterial nano fiber - Google Patents
A kind of preparation method based on polyelectrolyte surfactant complexes antibacterial nano fiber Download PDFInfo
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- CN110373735A CN110373735A CN201910585238.8A CN201910585238A CN110373735A CN 110373735 A CN110373735 A CN 110373735A CN 201910585238 A CN201910585238 A CN 201910585238A CN 110373735 A CN110373735 A CN 110373735A
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- polyelectrolyte
- surfactant
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of preparation methods based on polyelectrolyte surfactant complexes antibacterial nano fiber.This method comprises: obtaining polyelectrolyte high polymer for polyacrylonitrile hydrolyzed, then with surfactant quaternary ammonium salt self assembly, polyelectrolyte surfactant complexes are obtained, last electrostatic spinning obtains polyelectrolyte surfactant complexes antibacterial nano fiber.This method preparation route is simple, reaction condition is mild, at low cost, and nontoxic；Obtained nanofiber has preferably antibacterial effect and long-acting performance, while reducing subsequent arranging process, extends the application range of polyelectrolyte surfactant complexes.
Description
Technical field
The invention belongs to the preparation fields of antibacterial nano fiber, in particular to a kind of to be based on polyelectrolyte-surfactant
The preparation method of compound antibacterial nano fiber.
Background technique
Microorganism generates significant damage to human health and life, these microorganisms breed rapidly under the suitable conditions,
Transmission is carried out, the living environment of the mankind is influenced.Textile is the important medium for transmitting germ, can be provided to microorganism numerous
Grow the condition of life.Therefore research antibacterial fabric has great importance.Anti-bacterial fibre is a kind of with sterilization, bacteriostasis property
New function material, core component is anti-biotic material.The preparation of anti-bacterial fibre, which is specifically included that, makes antibacterial by physical method
Agent is mixed into fibrous inside, carries out chemical modification or grafting to the macromolecular structure of chemical fibre, utilizes composite spinning technology etc..
Electrostatic spinning technique is the simple and effective method of one kind for preparing antibiotic property nanofiber, electro spinning nano fiber tool
There is huge specific surface area, assigns its broad application prospect.Polyelectrolyte in weak solution with the surface-active of opposite charges
Agent can form solid material-polyelectrolyte surfactant complexes orderly on molecular level by molecular self-assembling.Research
Personnel have made compared with in-depth study the interaction in aqueous solution between the two, but to the polyelectrolyte-of solid-state structure
The research of surfactant complex is less, especially in terms of its functional application.The present invention is by polyelectrolyte and has antibiotic property
The quaternary cationic surfactant self assembly of energy obtains polyelectrolyte surfactant complexes, and passes through Static Spinning
Silk technology obtains antibacterial nano fiber, extends its application range.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to be received based on polyelectrolyte surfactant complexes antibacterial
The preparation method of rice fiber, extends the application range of polyelectrolyte surfactant complexes.
A kind of preparation method based on polyelectrolyte surfactant complexes antibacterial nano fiber of the invention, including
Will be polyacrylonitrile hydrolyzed, polyelectrolyte high polymer is obtained, then with surfactant quaternary ammonium salt self assembly, obtains polyelectrolyte-
Surfactant complex, last electrostatic spinning are obtained based on polyelectrolyte surfactant complexes antibacterial nano fiber.
A kind of preparation method based on polyelectrolyte surfactant complexes antibacterial nano fiber of the invention, specifically
Step includes:
(1) basic hydrolysis polyacrylonitrile (PAN) is used, PAN hydrolysate, i.e. anionic polyelectrolyte high polymer are obtained；
(2) anionic polyelectrolyte high polymer in step (1) is dissolved in deionized water, surfactant-season is slowly added dropwise
Ammonium salt aqueous solution, stirring, filtering, cleaning are dry, obtain polyelectrolyte surfactant complexes, wherein surfactant-
The mass ratio of quaternary ammonium salt and polyelectrolyte high polymer is 2:1；
(3) polyelectrolyte surfactant complexes in step (2) are dissolved in solvent, are stirred, the spinning solution that will be obtained
Electrostatic spinning is carried out, obtains wherein gathering electrolysis in spinning solution based on polyelectrolyte surfactant complexes antibacterial nano fiber
Matter-surfactant complex mass fraction is 10%.
Basic hydrolysis polyacrylonitrile (PAN) is used in the step (1) specifically: add PAN and sodium hydroxide for 1:1 with mass ratio
Enter into water, 100 DEG C of stirring 3h or more, precipitating, cleaning, drying obtain anionic polyelectrolyte high polymer.
The drying temperature is 40~60 DEG C.
Quaternary ammonium salt is dodecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecane in the step (2)
Base trimethyl ammonium chloride or octadecyltrimethylammonium chloride.
Whipping temp is 40~60 DEG C in the step (2), mixing time 30min.
It is dry in the step (2) are as follows: to be dried in vacuo at 40-60 DEG C.
Solvent is one of isopropanol, methylene chloride, chloroform or two kinds of mixing in the step (3).
Whipping temp is room temperature in the step (3), and mixing time is 6h or more.
The technological parameter of electrostatic spinning in the step (3) are as follows: application voltage is 10~20KV, and receiving distance is 10-
20cm, solution flow velocity are 0.5-1.0mL/h.
The present invention provides a kind of by the fine based on polyelectrolyte surfactant complexes antimicrobial nano of above method preparation
Dimension.
The present invention provides a kind of by the fine based on polyelectrolyte surfactant complexes antimicrobial nano of above method preparation
The application of dimension.
Nanofiber obtained in the present invention has preferably antibacterial effect and long-acting performance, while reducing subsequent arrangement
Process extends the application range of polyelectrolyte surfactant complexes.
Beneficial effect
In the present invention based on polyelectrolyte surfactant complexes antibacterial nano fiber have preferably antibacterial effect and
Long-acting performance, while reducing subsequent arranging process.In addition, technique preparation route of the invention is simple, reaction condition is mild, at
This is low and nontoxic.And prepared antibacterial nano fiber can be widely used in the fields such as biological, medical, weaving.
Detailed description of the invention
Fig. 1 is polyelectrolyte and electrostatic spinning nano fiber after dodecyl trimethyl ammonium chloride self assembly in embodiment 1
SEM electron microscope；
Fig. 2 is polyelectrolyte and electrostatic spinning nano fiber after tetradecyl trimethyl ammonium chloride self assembly in embodiment 2
SEM electron microscope；
Fig. 3 is polyelectrolyte and electrostatic spinning nano fiber after hexadecyltrimethylammonium chloride self assembly in embodiment 3
SEM electron microscope；
Fig. 4 is polyelectrolyte and hexadecyltrimethylammonium chloride electrostatic spinning nano fiber antibacterial effect figure in embodiment 3,
Wherein, a, d are respectively antibacterial effect of the blank sample to Escherichia coli (E.coli) and staphylococcus aureus (S.aureus)
Figure, b, e are respectively antibacterial effect figure of the PAN sample to Escherichia coli (E.coli) and staphylococcus aureus (S.aureus),
C, f is respectively antibacterial effect figure of the sample 16 to Escherichia coli (E.coli) and staphylococcus aureus (S.aureus)；
Fig. 5 is polyelectrolyte and electrostatic spinning nano fiber after octadecyltrimethylammonium chloride self assembly in embodiment 4
SEM electron microscope.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) preparation of polyelectrolyte high polymer:
10g sodium hydroxide is added into 200mL aqueous solution, after stirring and dissolving, is heated to 100 DEG C.It is poly- that 10g PAN high is added
Object powder, condensation stirring 3h.By acquired solution precipitating, cleaning, drying in 50 DEG C of baking oven is placed, obtains hydrolysis PAN high polymer,
That is polyelectrolyte high polymer.
(2) preparation of polyelectrolyte surfactant complexes:
4g polyelectrolyte is dissolved in 100mL deionized water, 8g dodecyl trimethyl ammonium chloride is dissolved in 200mL deionization
In water, then tenside/solvent is slowly dropped in polyelectrolyte solution until generating white precipitate, 50 DEG C are continued to stir
It mixes 30 minutes, the solution after reaction is filtered, cleaning, it is multiple to obtain polyelectrolyte-surfactant antibacterial for vacuum drying at 50 DEG C
Close object.
(3) preparation of polyelectrolyte surfactant complexes antibacterial nano fiber:
Polyelectrolyte surfactant complexes obtained by step (2) are dissolved in isopropanol and chloroform (the two volume ratio
For in 5:5), the spinning solution that configuration quality of materials score is 10% is stirred at room temperature 10 hours, carries out electrostatic spinning, applies voltage
For 11KV, receiving distance is 12cm, and solution flow velocity is 0.8mL/h.Obtained nano fibrous membrane is dried in vacuo 12h.Preparation
Submicron fiber film (being denoted as 12) is used for scanning electron microscope, and test results are shown in figure 1, can learn that fibre diameter is thicker, is in
Network structure.
Embodiment 2
" dodecyl trimethyl ammonium chloride " in 1 step of embodiment (3) is changed to " tetradecyl trimethyl ammonium chloride ",
Yu Jun is same as Example 1, obtains nano fibrous membrane.The submicron fiber film (being denoted as 14) of preparation is used for scanning electron microscope, surveys
Test result is as shown in Fig. 2, can learn that fibre diameter is thicker, in network structure.
Embodiment 3
" dodecyl trimethyl ammonium chloride " in 1 step of embodiment (3) is changed to " hexadecyltrimethylammonium chloride ",
Yu Jun is same as Example 1, obtains nano fibrous membrane.The submicron fiber film (being denoted as 16) of preparation is used for scanning electron microscope, surveys
Test result is as shown in figure 3, can learn that fibre diameter is thicker, in network structure.Electrostatic spinning nano fiber is to Escherichia coli
(E.coli) and the antibacterial effect of staphylococcus aureus (S.aureus) is as shown in Figure 4, it is seen that blank sample and the training of PAN sample
Bacterium mass propagation on ware is supported, without anti-microbial property.Sample 16 either to Escherichia coli or staphylococcus aureus, has
Preferable anti-microbial property, reaches 98% to the antibiotic rate of Escherichia coli, reaches 99% to the antibiotic rate of staphylococcus aureus.
Embodiment 4
" dodecyl trimethyl ammonium chloride " in 1 step of embodiment (3) is changed to " octadecyltrimethylammonium chloride ",
Yu Jun is same as Example 1, obtains nano fibrous membrane.The submicron fiber film (being denoted as 18) of preparation is used for scanning electron microscope, surveys
Test result is as shown in figure 5, can learn that fibre diameter is thicker, in network structure.
Claims (8)
1. a kind of preparation method based on polyelectrolyte surfactant complexes antibacterial nano fiber, comprising: by polyacrylonitrile
Hydrolysis, obtains polyelectrolyte high polymer, then with surfactant quaternary ammonium salt self assembly, obtains polyelectrolyte-surfactant
Compound, last electrostatic spinning are obtained based on polyelectrolyte surfactant complexes antibacterial nano fiber.
2. method according to claim 1, which is characterized in that it is described will be polyacrylonitrile hydrolyzed, obtain polyelectrolyte high polymer,
Then with surfactant quaternary ammonium salt self assembly, polyelectrolyte surfactant complexes are obtained, last electrostatic spinning obtains
Specific steps based on polyelectrolyte surfactant complexes antibacterial nano fiber include:
(1) basic hydrolysis polyacrylonitrile (PAN) is used, PAN hydrolysate, i.e. anionic polyelectrolyte high polymer are obtained；
(2) anionic polyelectrolyte high polymer in step (1) is dissolved in deionized water, surfactant-quaternary ammonium salt is slowly added dropwise
Aqueous solution, stirring, filtering, cleaning are dry, obtain polyelectrolyte surfactant complexes, wherein surfactant-quaternary ammonium
Salt and anionic polyelectrolyte high polymer mass ratio are 2:1；
(3) polyelectrolyte surfactant complexes in step (2) are dissolved in solvent, are stirred, obtained spinning solution is carried out
Electrostatic spinning obtains being based on polyelectrolyte surfactant complexes antibacterial nano fiber, wherein polyelectrolyte-in spinning solution
Surfactant complex mass fraction is 10%.
3. method according to claim 2, which is characterized in that specific with basic hydrolysis polyacrylonitrile (PAN) in the step (1)
Are as follows: PAN and sodium hydroxide are added to the water with mass ratio for 1:1,100 DEG C of stirring 3h or more, precipitating, cleaning are dried, obtained
Anionic polyelectrolyte high polymer.
4. method according to claim 2, which is characterized in that surfactant-quaternary ammonium salt is dodecane in the step (2)
Base trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecyltrimethylammonium chloride or octadecyl trimethyl chlorination
Ammonium；Whipping temp is 40~60 DEG C, mixing time 30min.
5. method according to claim 2, which is characterized in that solvent is isopropanol, methylene chloride, three in the step (3)
One of chloromethanes or two kinds of mixing；Whipping temp is room temperature, and mixing time is 6h or more.
6. method according to claim 2, which is characterized in that the technological parameter of electrostatic spinning in the step (3) are as follows: apply
Voltage is 10~20KV, and receiving distance is 10-20cm, and solution flow velocity is 0.5-1.0mL/h.
7. a kind of method as described in claim 1 preparation based on polyelectrolyte surfactant complexes antibacterial nano fiber.
8. a kind of method as described in claim 1 preparation based on polyelectrolyte surfactant complexes antibacterial nano fiber
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Cited By (3)
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| CN111518356A (en) * | 2020-05-20 | 2020-08-11 | 中国科学院长春应用化学研究所 | Modified polypropylene and preparation method thereof |
| CN113215727A (en) * | 2021-05-21 | 2021-08-06 | 南京工业大学 | Preparation method of air purification membrane with antibacterial property |
| CN114797503A (en) * | 2022-06-28 | 2022-07-29 | 南通纳爱斯环保科技有限公司 | Graphene-quaternary ammonium salt modified polyacrylonitrile composite fiber filtering membrane and preparation method thereof |
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| CN114797503A (en) * | 2022-06-28 | 2022-07-29 | 南通纳爱斯环保科技有限公司 | Graphene-quaternary ammonium salt modified polyacrylonitrile composite fiber filtering membrane and preparation method thereof |
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