CN109566649A - A kind of preparation method of nano silver composite antibacterial material - Google Patents
A kind of preparation method of nano silver composite antibacterial material Download PDFInfo
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- CN109566649A CN109566649A CN201811648728.XA CN201811648728A CN109566649A CN 109566649 A CN109566649 A CN 109566649A CN 201811648728 A CN201811648728 A CN 201811648728A CN 109566649 A CN109566649 A CN 109566649A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of preparation methods of nano silver composite antibacterial material, according to mass percent number meter: the concentrated nitric acid including 10%-40%, the Ag simple substance simple substance of 5%-20%, the sodium chloride of 10%-20%, the acidic catalyst of 0.2%-2%, the cationic surfactant of 15%-40%, the basic catalyst of 0.2%-2%, the solvent of 6%-50% and the tetraethyl orthosilicate of 0.6%-40%, proportionally, the concentrated nitric acid of 10%-40% and the Ag simple substance simple substance of 5%-20% are added into reaction kettle, dehydration obtains dispersion liquid after being thoroughly mixed, it will be protected from light in the cationic surfactant solution of 15%-40%, the sodium chloride of the resulting solution of the first step and 10%-20% is successively added dropwise to the sun of 15%-40% It is protected from light in cationic surfactant solutions, it is stirred to react, temperature is increased to 35-90 degree, persistently keep the temperature 5-12 hours, 60% cationic surfactant solution is added again into resulting solution, this anti-biotic material, which avoids, directly has that impurity causes the antibacterial effect of the anti-biotic material of preparation poor using the silver nitrate solution of long-term preservation, keeps the anti-microbial property of anti-biotic material obtained more lasting.
Description
Technical field
The present invention relates to the preparation technical field of anti-biotic material, specially a kind of preparation side of nano silver composite antibacterial material
Method.
Background technique
With the development and continuous improvement of people's living standards of society, the health that people gradually begin to focus on itself is asked
Topic, rhythm of life accelerates and the increase of population mobility, causes to breed more bacterium in environment, bacterium is increased to people's
Health causes serious influence, the method for existing sterilizing be usually to often in contact with component carry out high temperature, high pressure
Or ultraviolet light irradiation-sterilize etc..
One, the sterilizing range of existing high temperature, high pressure and ultraviolet light irradiation is more limited to, and cannot fundamentally be solved thin
Bacterium infection problems, and the implementation process of such sterilization mode is relatively complicated；
Two, anti-biotic material in the prior art typically directly adds the various medicaments with antibacterial action in the material, should
The antibacterial effect of class anti-biotic material is poor, and the antibacterial phase is limited, for this purpose, it is proposed that a kind of system of nano silver composite antibacterial material
Preparation Method.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of nano silver composite antibacterial material, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the invention provides the following technical scheme: a kind of nano silver composite antibacterial material, according to quality
Percentage number meter: the Ag simple substance of concentrated nitric acid, 5%-20%, the sodium chloride of 5%-20%, 0.2%-2% including 10%-40%
Acidic catalyst, the cationic surfactant of 15%-40%, the basic catalyst of 0.2%-2%, 6%-50% solvent
And the tetraethyl orthosilicate of 0.6%-40%, include the following steps:
(1) proportionally, the concentrated nitric acid of 10%-40% and the Ag simple substance simple substance of 5%-20% are added into reaction kettle, fills
Dehydration after being stirred is divided to obtain dispersion liquid；
(2) will be protected from light in the cationic surfactant solution of 15%-40%, by the resulting solution of the first step and
The sodium chloride of 10%-20% is successively added dropwise in the cationic surfactant solution of 15%-40% and is protected from light, and stirring is anti-
It answers, temperature is increased to 35-90 degree, persistently keep the temperature 5-12 hours；
(3) cationic surfactant solution of 15%-40% is added again into the resulting solution of second step, is added
The tetraethyl orthosilicate of the acidic catalyst of 0.2%-2%, the basic catalyst of a small amount of 0.2%-2% and 0.6%-40% into
Row reaction, temperature are continually maintained in 35-90 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, the solvent of 6%-50% is added by several times, then
It is protected from light dry to get the finished product for meeting anti-biotic material to nano silver.
Preferably, the cationic surfactant is dodecyl benzyl dimethyl ammonium chloride, dodecyldimethylamine base
One kind of benzyl ammonium chloride, cetalkonium chloride and stearyl dimethyl benzyl ammonium chloride.
Preferably, the acidic catalyst is one kind of hydrochloric acid or phosphoric acid.
Preferably, the basic catalyst is one kind of triethylamine, ammonium hydroxide and dicyandiamide.
Preferably, the interval time that the solvent of 6%-50% is added in the step 4 by several times is ten minutes.
Preferably, the solvent is one kind of ethyl alcohol, benzyl alcohol and ethylene glycol.
Preferably, the mixing time in the step 2 is 8-15min.
Preferably, the reaction time of the step 3 is 5-16 hours.
The beneficial effects of the present invention are: the present invention, which directly reacts silver-colored simple substance with concentrated nitric acid, is made silver nitrate solution, avoid
The direct silver nitrate solution using long-term preservation has that impurity causes the antibacterial effect of the anti-biotic material of preparation poor, by
Preferable in the antibacterial effect of Ag+, which is attached to Ag+ in the shell with porous silica, considerably increases Ag+
Stability, keep the anti-microbial property of anti-biotic material obtained more lasting, avoid the feelings of existing anti-biotic material anti-microbial property difference
Condition, structure is simple, convenient for operation and realizes.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of nano silver composite antibacterial material, according to mass percent number meter: mono- including 20% concentrated nitric acid, 10% Ag
Matter, 10% sodium chloride, 0.5% acidic catalyst, 50% cationic surfactant, 0.2% basic catalyst,
30% solvent and 3% tetraethyl orthosilicate；
Nano silver meet anti-biotic material the preparation method is as follows:
(1) proportionally, 20% concentrated nitric acid and 10% Ag simple substance are added into reaction kettle, after being thoroughly mixed
Dehydration obtains dispersion liquid；
(2) it will be protected from light in 50% cationic surfactant solution, by the resulting solution of the first step and 10% chlorination
Sodium is successively added dropwise in 50% cationic surfactant solution and is protected from light, and is stirred to react, and temperature is increased to 50 degree,
Persistently keep the temperature 6 hours；
(3) 50% cationic surfactant solution is added again into the resulting solution of second step, is added 0.5%
Acidic catalyst, 0.2% a small amount of basic catalyst and 3% tetraethyl orthosilicate reacted, temperature continues to keep
At 50 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, 30% solvent is added by several times, is then protected from light
Drying is to get the finished product for meeting anti-biotic material to nano silver.
Embodiment 2
A kind of nano silver composite antibacterial material, according to percentage number meter: including 25% concentrated nitric acid, 15% Ag simple substance,
13% sodium chloride, 1% acidic catalyst, 60% cationic surfactant, 0.4% basic catalyst, 40%
Solvent and 10% tetraethyl orthosilicate；
Nano silver meet anti-biotic material the preparation method is as follows:
(1) proportionally, 25% concentrated nitric acid and 15% Ag simple substance are added into reaction kettle, after being thoroughly mixed
Dehydration obtains dispersion liquid；
(2) it will be protected from light in 60% cationic surfactant solution, by the resulting solution of the first step and 13% chlorination
Sodium is successively added dropwise in 60% cationic surfactant solution and is protected from light, and is stirred to react, and temperature is increased to 62 degree,
Persistently keep the temperature 8 hours；
(3) 50% cationic surfactant solution is added again into the resulting solution of second step, is added 0.5%
Acidic catalyst, 0.4% a small amount of basic catalyst and 10% tetraethyl orthosilicate reacted, temperature continues to keep
At 62 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, 30% solvent is added by several times, is then protected from light
Drying is to get the finished product for meeting anti-biotic material to nano silver.
Embodiment 3
A kind of nano silver composite antibacterial material, according to percentage number meter: including 35% concentrated nitric acid, 17% Ag simple substance,
16% sodium chloride, 1.4% acidic catalyst, 40% cationic surfactant, 0.6% basic catalyst, 50%
Solvent and 20% tetraethyl orthosilicate；
Nano silver meet anti-biotic material the preparation method is as follows:
(1) proportionally, 35% concentrated nitric acid and 17% Ag simple substance are added into reaction kettle, after being thoroughly mixed
Dehydration obtains dispersion liquid；
(2) it will be protected from light in 40% cationic surfactant solution, by the resulting solution of the first step and 16% chlorination
Sodium is successively added dropwise in 80% cationic surfactant solution and is protected from light, and is stirred to react, and temperature is increased to 80 degree,
Persistently keep the temperature 10 hours；
(3) 40% cationic surfactant solution is added again into the resulting solution of second step, is added 1.4%
Acidic catalyst, 0.6% a small amount of basic catalyst and 20% tetraethyl orthosilicate reacted, temperature continues to keep
At 80 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, 30% solvent is added by several times, is then protected from light
Drying is to get the finished product for meeting anti-biotic material to nano silver.
Embodiment 4
A kind of nano silver composite antibacterial material, according to percentage number meter: including 40% concentrated nitric acid, 20% Ag simple substance,
20% sodium chloride, 2% acidic catalyst, 38% cationic surfactant, 1% basic catalyst, 50% it is molten
Agent and 40% tetraethyl orthosilicate；
Nano silver meet anti-biotic material the preparation method is as follows:
(1) proportionally, 40% concentrated nitric acid and 20% Ag simple substance are added into reaction kettle, after being thoroughly mixed
Dehydration obtains dispersion liquid；
(2) it will be protected from light in 38% cationic surfactant solution, by the resulting solution of the first step and 20% chlorination
Sodium is successively added dropwise in 38% cationic surfactant solution and is protected from light, and is stirred to react, and temperature is increased to 90 degree,
Persistently keep the temperature 12 hours；
(3) 38% cationic surfactant solution is added again into the resulting solution of second step, is added 1.4%
Acidic catalyst, 1% a small amount of basic catalyst and 40% tetraethyl orthosilicate reacted, temperature is continually maintained in
90 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, 50% solvent is added by several times, is then protected from light
Drying is to get the finished product for meeting anti-biotic material to nano silver.
Test case 1
Anti-microbial property test:
It takes common anti-biotic material plate and the nano silver obtained to meet anti-biotic material plate and distinguishes one, place it in temperature
To sterilize in 200 degree of high-temperature water, then in rubber head dropper bacterium solution drop respectively two anti-biotic materials of dropwise addition of equivalent, bedding is thin
Film makes bacterium solution uniformly be coated in sample surfaces, waits 10 hours.
Control group is the common anti-biotic material plate of uncoated coating.
Antibacterial experiment uses film adhesion method, to two kinds of common microorganism-Gram-positive S staphylococcuses and leather
Lan Shi negative bacterium is detected.
Test method is as follows:
Beef extract 0.3g and peptone 0.5g are blended in 100mL water, Broth solution is made, by staphylococcus aureus
With each colony inoculation of Escherichia coli into the meat soup of 20mL.In 37 DEG C of shaking tables for 24 hours with the speed culture of 150rpm, so
Bacteria suspension is diluted with 0.85% sterile NaCl solution afterwards.
Common anti-biotic material and nano silver obtained are met into anti-biotic material plate and are respectively put into 37 DEG C of culture 3h of bacteria suspension
Afterwards, nano silver antibacterial material plate is added in agarose plate, 37 DEG C of cultures count for 24 hours.
As a result as shown in the table:
According to upper table, a kind of nano silver composite antibacterial material of the present invention has good antibiotic property, contacts with bacterium
After 5h, the clump count of two kinds of bacteriums is constantly reduced.
Test case 2
The anti-microbial property test of nano silver attachment different materials:
Common nano silver antibacterial material plate and the Ag+ obtained is taken to adhere to the anti-biotic material plate point of porous silica shell
Other one, the two anti-biotic material plates are separately immersed in certain density bacterium solution constantly shake culture, are waited 10 hours.
Control group is common nano silver antibacterial material plate.
Antibacterial experiment uses succusion, to two kinds of common microorganism-Gram-positive S staphylococcuses and gram
Negative bacterium is detected.
Test method is as follows:
Beef extract 0.3g and peptone 0.5g are blended in 100mL water, Broth solution is made, by staphylococcus aureus
With each colony inoculation of Escherichia coli into the meat soup of 20mL.In 37 DEG C of shaking tables for 24 hours with the speed culture of 150rpm, so
Bacteria suspension is diluted with 0.85% sterile NaCl solution afterwards.
Common nano silver antibacterial material plate and Ag+ obtained are adhered to the anti-biotic material plate of the shell of porous silica
After being respectively put into 37 DEG C of culture 3h of bacteria suspension, nano silver antibacterial material plate is added in agarose plate, 37 DEG C of cultures are counted for 24 hours
Number.
As a result as shown in the table:
According to upper table, the anti-biotic material plate that a kind of Ag+ of the present invention adheres to the shell of porous silica has good
Good antibiotic property, after contacting 5h with bacterium, the clump count of two kinds of bacteriums is constantly reduced.
Claims (8)
1. a kind of nano silver composite antibacterial material, which is characterized in that according to mass percent number meter: the dense nitre including 10%-40%
The cation surface activating of acid, the acidic catalyst of the Ag simple substance of 5%-20%, the sodium chloride of 5%-20%, 0.2%-2%, 15%-40%
Agent, the basic catalyst of 0.2%-2%, the solvent of 6%-50% and 0.6%-40% tetraethyl orthosilicate；
Nano silver meet anti-biotic material the preparation method is as follows:
(1) proportionally, the concentrated nitric acid of 10%-40% and the Ag simple substance simple substance of 5%-20% are added into reaction kettle, is sufficiently stirred mixed
Dehydration obtains dispersion liquid after conjunction；
(2) it will be protected from light in the cationic surfactant solution of 15%-40%, by the chlorine of the first step resulting solution and 10%-20%
Change sodium, which is successively added dropwise in the cationic surfactant solution of 15%-40%, to be protected from light, and is stirred to react, temperature is increased to
35-90 degree persistently keeps the temperature 5-12 hours；
(3) cationic surfactant solution of 15%-40% is added again into the resulting solution of second step, 0.2%-2% is added
Acidic catalyst, the basic catalyst of a small amount of 0.2%-2% and the tetraethyl orthosilicate of 0.6%-40% reacted, temperature after
It is continuous to be maintained at 35-90 degree；
(4) final solution obtained in third step is subjected to centrifugal treating, the solvent of 6%-50% is added by several times, is then protected from light dry
It is dry to get the finished product for meeting anti-biotic material to nano silver.
2. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: it is described sun from
Sub- surfactant is dodecyl benzyl dimethyl ammonium chloride, myristyl benzyl dimethyl ammonium chloride, etradecyldimethylamine
One kind of base benzyl ammonium chloride and stearyl dimethyl benzyl ammonium chloride.
3. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the acidity
Catalyst is one kind of hydrochloric acid or phosphoric acid.
4. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the alkalinity
Catalyst is one kind of triethylamine, ammonium hydroxide and dicyandiamide.
5. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the step
The interval time that the solvent of 6%-50% is added in four by several times is ten minutes.
6. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the solvent
For one kind of ethyl alcohol, benzyl alcohol and ethylene glycol.
7. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the step
Mixing time in two is 8-15min.
8. a kind of preparation method of nano silver composite antibacterial material according to claim 1, it is characterised in that: the step
Three reaction time is 5-16 hours.
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| CN201811648728.XA CN109566649A (en) | 2018-12-30 | 2018-12-30 | A kind of preparation method of nano silver composite antibacterial material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202091A (en) * | 2020-01-08 | 2020-05-29 | 华南理工大学 | Nano-silver loaded mesoporous silica antibacterial material and preparation method and application thereof |
| CN112846216A (en) * | 2021-01-06 | 2021-05-28 | 江苏新日电动车股份有限公司 | Method for preparing stable compound by gas-liquid plasma technology and application thereof |
-
2018
- 2018-12-30 CN CN201811648728.XA patent/CN109566649A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202091A (en) * | 2020-01-08 | 2020-05-29 | 华南理工大学 | Nano-silver loaded mesoporous silica antibacterial material and preparation method and application thereof |
| CN112846216A (en) * | 2021-01-06 | 2021-05-28 | 江苏新日电动车股份有限公司 | Method for preparing stable compound by gas-liquid plasma technology and application thereof |
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Application publication date: 20190405 |