CN110343327A - A kind of chitosan loaded nanometer silver antimicrobial polypropylene material and preparation method thereof - Google Patents
A kind of chitosan loaded nanometer silver antimicrobial polypropylene material and preparation method thereof Download PDFInfo
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- CN110343327A CN110343327A CN201910654756.0A CN201910654756A CN110343327A CN 110343327 A CN110343327 A CN 110343327A CN 201910654756 A CN201910654756 A CN 201910654756A CN 110343327 A CN110343327 A CN 110343327A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of chitosan loaded nanometer silver antimicrobial polypropylene materials and preparation method thereof, belong to polymer modification field.The antibacterial polypropylene material includes acrylic resin and support type antibacterial agent, wherein support type antibacterial agent is 0.1 ~ 30 parts by weight in terms of being 100 parts by weight by acrylic resin；The support type antibacterial agent is chitosan/nano silver composite antibacterial agent, and wherein nano-silver loaded is on chitosan, and the mass ratio of nano silver and chitosan is 1/100-100/100.The advantages that complex antimicrobials of the present invention have dosage few, environmentally protective, cheap, and anti-microbial property is lasting, not only anti-microbial property is excellent for thus obtained antibacterial polypropylene material, but also its mechanical property is improved.In addition to this, antibacterial polypropylene material preparation process is simple, easily operated, is suitable for industrial applications, has very high economy and society value.
Description
Technical field
The invention belongs to polymer modification fields, further say, are that be related to a kind of chitosan loaded nano silver anti-
Bacterium polypropylene material and preparation method thereof, the antibacterial polypropylene can be applied to the various fields for producing and living.
Background technique
With the development of economy, improvement of living standard, demand of the people to anti-biotic material have extended to all kinds of fields, at
For indispensable a part in producing and living.Polypropylene is as one of five big general-purpose plastics, because of its excellent mechanical performance
And the advantages that processing performance, and it is widely used in the numerous areas such as daily necessity, medical machinery, household electrical appliances, building materials and packaging.Cause
This, develops the hot spot that antibacterial polypropylene material is always antibacterial field.
Antibacterial agent is the core of anti-biotic material, generally assigns material and then adding a small amount of antibacterial agent in plastic products
Expect anti-microbial property, makes it have sterilization or bacteriostasis.Currently, the ingredient according to antibacterial agent is different, can be classified as inorganic anti-
Microbial inoculum, organic antibacterial agent, natural antibacterial agent three categories.Inorganic antiseptic is mainly by ion-exchange, physisorphtion, chemistry
Absorption method is carrier by some materials with Kong Jie such as diatomite, zeolite, apatite etc., with the metal for having bacteriostasis property
Ion such as zinc, silver, copper ion, which combine, to be made.In a series of inorganic antiseptics, silver-series antibacterial agent is due to has a broad antifungal spectrum, resisting
The features such as bacterium persistent, safety, extremely low drug resistance, it has also become antibacterial and the main direction of development.Organic antibacterial agent is mostly
The substances such as the organic matter of some specific structures and types of radicals, including quaternary ammonium salt, biguanides, alcohols.And natural antibacterial agent is
The antibacterial agent that the mankind use earliest derives from the Nature, is mainly obtained by driven plant extract, purifying, is a kind of advantageous
In the antibacterial agent of environment, the most commonly used is chitosans.
Difference of all kinds of antibacterial agents according to preparation method, processing performance, anti-microbial property etc., shows respective excellent
Disadvantage.For example, inorganic antiseptic is heat-resist, have the characteristics that excellent broad-spectrum antibacterial property and persistence, but it is in product
In be easily precipitated, and product is made to change colour；And natural antibacterial agent is nontoxic to the human body, non-stimulated, it is safe to use, but chitosan class
Natural antibacterial agent antibacterial activity is low, and cannot be directly dissolved in water and ordinary organic solvents, makes its application range by the very day of one's doom
System.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of chitosan loaded nanometer silver antimicrobial polypropylene
Material and preparation method thereof, while a kind of chitosan/nano silver composite antibacterial agent being provided, the antibacterial polypropylene material not only resists
Bacterium significant effect, antibacterial time is more longlasting, and preparation process is simple, and mechanical property is also improved.
In order to achieve the above objectives, the present invention is achieved by the following technical solutions:
A kind of chitosan loaded nanometer silver antimicrobial polypropylene material, raw material composition include that acrylic resin and support type are anti-
Microbial inoculum, wherein by acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 0.1~30 parts by weight；The support type antibacterial
Agent is chitosan/nano silver composite antibacterial agent, and wherein nano-silver loaded is on chitosan, and the mass ratio of nano silver and chitosan
For 1/100-100/100.
Further, the chitosan loaded nanometer silver antimicrobial polypropylene material, raw material are formed with acrylic resin
For 100 parts by weight meters, support type antibacterial agent is 0.3~15 parts by weight.
Further, the acrylic resin is one of homopolypropylene, copolymer polypropylene or their combination
Object.
Further, the chitosan/nano silver composite antibacterial agent the preparation method comprises the following steps:
(1) a certain amount of chitosan is added after ultrapure water being heated with stirring to 80-100 DEG C, chitosan suspension is prepared
Liquid；
(2) a certain amount of AgNO3 solution is added in chitosan suspension described in step (1)；
(3) reducing agent is added in the mixed solution of step (2), continues to be cooled to room temperature after stirring 10min, separate, uses
Milli-Q water is dried in vacuo 18 hours under the conditions of 60-70 DEG C to get chitosan/nano silver composite antibacterial agent.
Reducing agent described in step (3) is the mixed of one or more of ethylene glycol, glucose, chitosan etc. substance
Close object.
In chitosan obtained by step (3)/nano silver composite antibacterial agent, the mass ratio of nano silver and chitosan is 5/
100-50/100。
The present invention also provides the preparation method of the chitosan loaded nanometer silver antimicrobial polypropylene material, feature exists
In: the acrylic resin centainly matched and chitosan/nano silver composite antibacterial agent are uniformly mixed in super mixer, then
By mixture through double screw extruder extruding pelletization, extrusion process are as follows: 180 DEG C of area's temperature, two 210 DEG C of area's temperature, three Qu Wen
210 DEG C of degree, four 210 DEG C of area's temperature, five 210 DEG C of area's temperature, six 180 DEG C of area's temperature, charging rate 5r/min, discharging speed 15r/
min；Then gained antibacterial polypropylene particle is dried in vacuo 24 hours under the conditions of 60-70 DEG C, the chitosan for being made described is negative
Carrying nano silver antibacterial polypropylene material.
Further, the acrylic resin and chitosan/nano silver composite antibacterial agent mass ratio be 100/0.3~
100/15。
In addition, chitosan prepared by the present invention/nano silver composite antibacterial agent, is applicable not only to polypropylene material, may be used also
The matrixes such as ABS resin, polystyrene, polyamide, polyformaldehyde, polyester are added and prepare anti-biotic material.
The present invention is by improving traditional formula, and using natural polymer chitosan as carrier, loading nano silvery is inorganic anti-
Microbial inoculum can not only retain silver and the original performance of polymeric matrix, and obtain performance not available for stock blend.On the one hand,
Hydroxyl and amido functional group in chitosan molecule chain can stablize nano silver, play buffering releasing effect to nano silver, so that
Antibacterial time is more longlasting.In addition, chitosan and polypropylene have good compatibility, it not only can guarantee that nano silver is being moulded
Good dispersibility in material products, and also improve the stability and persistence of antibacterial agent.On the other hand, the addition of nano silver
Can overcome chitosan anti-bacteria activity it is low and can only contact it is antibacterial the disadvantages of, expand its application range.In addition to chitosan with
Learning from other's strong points to offset one's weaknesses between nano silver, the addition of the support type antibacterial agent can also simplify the preparation process of antibacterial polypropylene material,
And improve the mechanical property of polypropylene material.
The beneficial effects of the present invention are:
(1) using natural polymer chitosan as carrier, loading nano silvery inorganic antiseptic plays buffering to nano silver and releases
Effect is put, so that antibacterial time is more longlasting.
(2) chitosan and polypropylene have good compatibility, guarantee nano silver good dispersibility in plastic products,
The antibacterial stability and persistence of material are improved simultaneously.
(3) nano silver and chitosan are all antibacterial agent, antibacterial activity not only can be improved by the two is compound, but also can expand
The application range of big anti-biotic material.
(4) chitosan is environmentally protective, from a wealth of sources, cheap as natural macromolecular material, can suitably subtract in this way
The use of few nano silver, reduces the cost of antibacterial polypropylene material, improves its biological safety.
(5) chitosan loaded nano silver antimicrobials can be directly added into polypropylene matrix and prepares anti-biotic material, without system
Standby antibacterial matrices, preparation process is simple, is conducive to large-scale industrial production.
Detailed description of the invention
Fig. 1 is that the SEM of chitosan loaded nano silver antimicrobials schemes；
Fig. 2 is that the UV-vis of chitosan loaded nano silver antimicrobials schemes；
Fig. 3 is the XRD diagram of chitosan loaded nano silver antimicrobials；
Fig. 4 is the antibacterial effect figure of virgin pp and chitosan loaded nanometer silver antimicrobial polypropylene material to Escherichia coli；
Fig. 5 is that virgin pp and chitosan loaded nanometer silver antimicrobial polypropylene material imitate the antibacterial of staphylococcus aureus
Fruit figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited solely to following embodiment
And implementation method.
Embodiment 1
A kind of chitosan loaded nanometer silver antimicrobial polypropylene material, raw material composition include acrylic resin and homemade load
Type antibacterial agent, wherein by acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 8 parts；The support type antibacterial agent is shell
Glycan/nano silver composite antibacterial agent, wherein nano-silver loaded is on chitosan, and the mass ratio of nano silver and chitosan is 5/
100。
The chitosan/nano silver composite antibacterial agent the preparation method comprises the following steps:
(1) 0.1g chitosan is added after 50ml ultrapure water being heated with stirring to 90 DEG C, chitosan suspension is prepared；
(2) AgNO for being 0.1mol/L by 0.5ml concentration3Solution is added in chitosan suspension described in step (1)；
(3) 0.5mg glucose is added in the mixed solution described in step (2), continues to be cooled to room after stirring 10min
Temperature, separation, with milli-Q water 5 times, is dried in vacuo 18 hours under the conditions of 70 DEG C to get chitosan/nano silver composite antibacterial
Agent.
A kind of preparation method of chitosan loaded nanometer silver antimicrobial polypropylene material, includes the following steps: to match and is
100/8 acrylic resin and chitosan/nano silver composite antibacterial agent is uniformly mixed in super mixer, then by mixture
Through double screw extruder extruding pelletization, extrusion process are as follows: 180 DEG C of area's temperature, two 210 DEG C of area's temperature, three 210 DEG C of area's temperature,
Four 210 DEG C of area's temperature, five 210 DEG C of area's temperature, six 180 DEG C of area's temperature, charging rate 5r/min, discharging speed 15r/min；Then
Antibacterial polypropylene particle is dried in vacuo 24 hours under the conditions of 70 DEG C, the chitosan loaded nanometer silver antimicrobial poly- third is made
Alkene material.
Embodiment 2
Except the reducing agent prepared in chitosan/nano silver composite antibacterial agent step (3) is adjusted to 0.5ml ethylene glycol solution
Outside, other processing steps are same as Example 1.
Embodiment 3
A kind of chitosan loaded nanometer silver antimicrobial polypropylene material, raw material composition include acrylic resin and homemade load
Type antibacterial agent, wherein by acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 8 parts；The support type antibacterial agent is shell
Glycan/nano silver composite antibacterial agent, wherein nano-silver loaded is on chitosan, and the mass ratio of nano silver and chitosan is 20/
100。
The chitosan/nano silver composite antibacterial agent the preparation method comprises the following steps:
(1) 0.1g chitosan is added after 50ml ultrapure water being heated with stirring to 90 DEG C, chitosan suspension is prepared；
(2) AgNO for being 0.1mol/L by 2ml concentration3Solution is added in chitosan suspension described in step (1)；
(3) 0.5mg glucose is added in the mixed solution described in step (2), continues to be cooled to room after stirring 10min
Temperature, separation, with milli-Q water 5 times, is dried in vacuo 18 hours under the conditions of 70 DEG C to get chitosan/nano silver composite antibacterial
Agent.
The preparation method is the same as that of Example 1 for a kind of chitosan loaded nanometer silver antimicrobial polypropylene material.
Embodiment 4
A kind of chitosan loaded nanometer silver antimicrobial polypropylene material, raw material composition include acrylic resin and homemade load
Type antibacterial agent, wherein by acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 10 parts；The support type antibacterial agent is
Chitosan/nano silver composite antibacterial agent, wherein nano-silver loaded is on chitosan, and the mass ratio of nano silver and chitosan is 5/
100。
The chitosan/the preparation method is the same as that of Example 1 for nano silver composite antibacterial agent.
A kind of preparation method of chitosan loaded nanometer silver antimicrobial polypropylene material, includes the following steps: to match and is
100/10 acrylic resin and chitosan/nano silver composite antibacterial agent is uniformly mixed in super mixer, then will mixing
Object is through double screw extruder extruding pelletization, extrusion process are as follows: 180 DEG C of area's temperature, two 210 DEG C of area's temperature, three area's temperature 210
DEG C, four 210 DEG C of area's temperature, five 210 DEG C of area's temperature, six 180 DEG C of area's temperature, charging rate 5r/min, discharging speed 15r/min；
Then antibacterial polypropylene particle is dried in vacuo 24 hours under the conditions of 70 DEG C, the chitosan loaded nanometer silver antimicrobial is made
Polypropylene material.
Comparative example 1
Any antibacterial agent and auxiliary agent are not added, by 100 parts of acrylic resin powders through double screw extruder extruding pelletization, are squeezed
Technique out are as follows: 180 DEG C of area's temperature, two 210 DEG C of area's temperature, three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five area's temperature 210
DEG C, six 180 DEG C of area's temperature, charging rate 5r/min, discharging speed 15r/min；Then by PP GRANULES under the conditions of 70 DEG C
Vacuum drying 24 hours.
Comparative example 2
Other antibacterial agents and auxiliary agent are not added, by 100 parts of acrylic resin powders and 8 parts of chitosans in super mixer
It is uniformly mixed, then by mixture through double screw extruder extruding pelletization, extrusion process are as follows: 180 DEG C of area's temperature, two area's temperature
210 DEG C, three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five 210 DEG C of area's temperature, six 180 DEG C of area's temperature, charging rate 5r/min,
Discharging speed 15r/min；Then PP GRANULES is dried in vacuo 24 hours under the conditions of 70 DEG C.
Performance evaluation mode and implementation standard:
The drying particulate prepared by embodiment and comparative example method is subjected to injection moulding sample preparation in injector.
Tensile property test: it is carried out referring to national standard " plastic tensile performance test methods " (GB/T1040-92), using dumbbell
Type sample is tested at room temperature.
Impact property test: carrying out referring to national standard " plastics charpy impact test method " (GB/T1043-93), using scarce
Oral examination sample is tested at room temperature.
Anti-microbial property test: referring to People's Republic of China's light industry standard " antibiotic plastic Anti-microbial Performance Tests method
And antibacterial effect " (QB/T 2591-2003) progress, it is tested using film applicator coating；Detect strain: staphylococcus aureus
(Staphylococcus aureus)ATCC 6538；Escherichia coli (Escherichiacoli) ATCC 25922.
Antibacterial resistance to persistence test: referring to Japan Antibacterial Products Technology Association " antibacterial fabricated product antimicrbial power duration examination
Test method " (2001 editions) progress, the specific steps are as follows: the polypropylene material in embodiment 1-4 and comparative example 1-2 is molded system respectively
At print, above-mentioned print is impregnated in deionized water, controls 55 DEG C of water temperature, soaking time 16h, is then tested using film applicator coating
The anti-microbial property of print.
The mechanics and anti-microbial property of table 1 embodiment 1-4 and comparative example 1-2 product
As can be seen from the above table, antibacterial polypropylene material prepared by the present invention not only has efficient anti-microbial property and excellent
Durability of antimicrobial effect, and be added chitosan/nano silver composite antibacterial agent after, the mechanical property of polypropylene material is also improved
It improves.
Fig. 1 is chitosan described in embodiment 1/nano silver composite antibacterial agent SEM figure, white as we can see from the figure to receive
Rice Argent grain is dispersed in chitosan surface, shows AgNO3Silver ion in solution is successfully restored and is carried on chitin carrier
On.
Fig. 2 is the UV-vis spectrogram of silver nitrate aqueous solution and the antibacterial agent using the preparation of different reducing agents, by bent in figure
Line can see, and characteristic peak does not occur near 400nm in silver nitrate solution, and other three groups of chitosan/nano silvers are compound anti-
There is characteristic ultraviolet absorption peak at 410nm in microbial inoculum, shows in three groups of antibacterial agents with the presence of nano silver particles.
Fig. 3 is chitosan described in pure chitosan and embodiment 1/nano silver composite antibacterial agent XRD diagram, can from figure
There is the peak crystallization of a nano silver at 38 ° in antibacterial agent out, and other several peak crystallizations of nano silver can't see, it should be
By the interference of chitosan, but it equally can determine that the presence for having nano silver in antibacterial agent.
Fig. 4 is that antibacterial polypropylene material described in virgin pp described in comparative example 1 and embodiment 1 imitates the antibacterial of Escherichia coli
Fruit figure, as can be seen from the figure density of the Escherichia coli after virgin pp culture on agar medium is very big, says
Bright virgin pp does not have antibacterial effect to Escherichia coli.And the Escherichia coli Jing Guo antibacterial polypropylene material culture are trained in agar
Almost all death on base is supported, illustrates that there is excellent antibiotic property to Escherichia coli by antibacterial polypropylene material prepared by the present invention
Energy.
Fig. 5 is antibacterial polypropylene material described in virgin pp described in comparative example 1 and embodiment 1 to staphylococcus aureus
Antibacterial effect figure, thus figure is as can be seen that antibacterial polypropylene material still has efficient antibacterial for staphylococcus aureus
Performance.
Particular embodiments described above for explaining only the invention, does not constitute any limitation of the invention, it is all
Made change, replacement, modification etc. under spirit and scope of the present invention are not departed from, is all covered by the present invention.
Claims (10)
1. a kind of chitosan loaded nanometer silver antimicrobial polypropylene material, it is characterised in that: its raw material composition includes acrylic resin
With support type antibacterial agent, wherein by acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 0.1 ~ 30 parts by weight；It is described
Support type antibacterial agent is chitosan/nano silver composite antibacterial agent, and wherein nano-silver loaded is on chitosan, and nano silver and shell are poly-
The mass ratio of sugar is 1/100-100/100.
2. chitosan loaded nanometer silver antimicrobial polypropylene material according to claim 1, it is characterised in that: its raw material composition
By acrylic resin be 100 parts by weight in terms of, support type antibacterial agent be 0.3 ~ 15 parts by weight.
3. chitosan loaded nanometer silver antimicrobial polypropylene material according to claim 1, it is characterised in that: the polypropylene
Resin is one of homopolypropylene, copolymer polypropylene or their compositions.
4. chitosan loaded nanometer silver antimicrobial polypropylene material according to claim 1, it is characterised in that: the shell is poly-
Sugar/nano silver composite antibacterial agent the preparation method comprises the following steps:
A certain amount of chitosan is added after water is heated with stirring to 80-100 DEG C, chitosan suspension is prepared；
By a certain amount of AgNO3Solution is added in chitosan suspension described in step (1)；
Reducing agent is added in the mixed solution of step (2), is cooled to room temperature after continuing stirring, separates, is washed with water, in 60-
Vacuum drying is under the conditions of 70 DEG C to get chitosan/nano silver composite antibacterial agent.
5. the preparation method of chitosan loaded nanometer silver antimicrobial polypropylene material according to any one of claims 1-4, special
Sign is: the acrylic resin centainly matched and chitosan/nano silver composite antibacterial agent is uniformly mixed in super mixer,
Then by mixture through double screw extruder extruding pelletization, extrusion process are as follows: 180 DEG C of area's temperature, two 210 DEG C of area's temperature,
Three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five 210 DEG C of area's temperature, six 180 DEG C of area's temperature, 5 r/min of charging rate,
15 r/min of discharging speed；Then gained antibacterial polypropylene particle is dried in vacuo under the conditions of 60-70 DEG C, is made described
Chitosan loaded nanometer silver antimicrobial polypropylene material.
6. the preparation method of chitosan loaded nanometer silver antimicrobial polypropylene material according to claim 5, it is characterised in that:
The acrylic resin and chitosan/nano silver composite antibacterial agent mass ratio are 100/0.3 ~ 100/15.
7. a kind of chitosan/nano silver composite antibacterial agent preparation method, it is characterised in that: itself the following steps are included:
(1) a certain amount of chitosan is added after water being heated with stirring to 80-100 DEG C, chitosan suspension is prepared；
(2) by a certain amount of AgNO3Solution is added in chitosan suspension described in step (1)；
(3) reducing agent is added in the mixed solution of step (2), is cooled to room temperature after continuing stirring, separate, be washed with water,
It is dried in vacuo under the conditions of 60-70 DEG C to get the chitosan/nano silver composite antibacterial agent, nano silver in the complex antimicrobials
Mass ratio with chitosan is 1/100-100/100.
8. chitosan according to claim 7/nano silver composite antibacterial agent preparation method, it is characterised in that: step (3)
The reducing agent is the mixture of one or more of ethylene glycol, glucose, chitosan substance.
9. a kind of chitosan obtained according to claim 7 or 8 the methods/nano silver composite antibacterial agent.
10. chitosan as claimed in claim 9/nano silver composite antibacterial agent application, it is characterised in that: poly- in the shell
Matrix is added in sugar/nano silver composite antibacterial agent, is used to prepare anti-biotic material, described matrix be acrylic resin, ABS resin,
Polystyrene, polyamide, polyformaldehyde or polyester.
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Application publication date: 20191018 |