CN1817138A - Silver-carried antibacterial agent with nanometer porous and making method thereof - Google Patents
Silver-carried antibacterial agent with nanometer porous and making method thereof Download PDFInfo
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- CN1817138A CN1817138A CN 200610024773 CN200610024773A CN1817138A CN 1817138 A CN1817138 A CN 1817138A CN 200610024773 CN200610024773 CN 200610024773 CN 200610024773 A CN200610024773 A CN 200610024773A CN 1817138 A CN1817138 A CN 1817138A
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Abstract
A nano-class mesoporous Ag-carried antibacterial agent used for detergent, cosmetics, water treating, textile, etc contains inorganic oxide as carrier with orderly mesopore structure and Ag as active antibacterial component. Its advantages are large specific surface area, broad spectrum, high effect and durability, and no damage to people.
Description
Technical field
The present invention relates to a kind of antibacterial agent and preparation method thereof, relate in particular to mesoporous carrying silver antimicrobials of a kind of novel nano and preparation method thereof.
Background technology
Current, environmental problem is severe day by day, and infectious disease is wreaked havoc, and human health is constituted greatly dangerous.Endangering bigger mainly is hepatitis viruse, influenza virus, AIDS virus, variability tuberculosis germ.According to the Ministry of Public Health 2003 statistics, in China, the carrier of hepatitis B surpasses 2.5 hundred million, the sexually infected person surpasses 1,300,000, tuberculosis patient surpasses 8,500,000 people, and the SARS in the first half of the year in 2003 has shocked the world especially.Whole world aids infection every day person reaches 10000 people above (the Asia ascendant trend is the fastest), annual influenza infection people (inferior) is hundreds of millions of.Many bacteriums in the food also are the roots that causes human body ill, are carcinogenic sources as some black bacterium and red bacterium, and pathogenicity colon bacillus, yellow staphylococcus, salmonella are the roots that causes food poisoning and disease propagation.Because these viruses and bacterium great majority are propagated by communal facility and article, in the daily life, people contact inevitably by virus or various article that bacterium polluted, thereby cause the generation of disease.Along with human living standard's raising, health care consciousness also strengthens gradually, also just requires comfortable safe living environment naturally.Therefore, the antimicrobial product of development and exploitation high-efficient and lasting is effectively killed and inhibition causes disease poison and bacterium, is the problem that the government department and the public press for solution.
Existing antimicrobial product can be divided into organic, natural and inorganic three big series.Studies show that the organic antibacterial agent heat-resisting quantity is poor, antibiotic long-lasting not good, and harmful, be eliminated gradually; Natural antibacterial agent has advantages such as antimicrobial efficiency height and safety non-toxic, but poor heat resistance, duration of efficacy is short, and resource-constrained; Inorganic antiseptic is because easily industrialization, and heat resistance and has a broad antifungal spectrum, performance is good and gain great popularity.The main component of inorganic antiseptic is support type gold, silver, zinc or copper etc., and the most frequently used is the Ag series antibacterial agent.Developed in succession at present with the inorganic antiseptic as carrier such as zeolite, apatite, titanium oxide, basic zirconium phosphate, silica gel, glass, clay pit, aluminium oxide and zeolite.But the major defect of its existence is: the particle diameter of (1) antibacterial agent is generally at 0.5～10 micron, can be less with the surface area that germ or bacterium contact, and the metal ion of antibiotic effective ingredient is at the skewness of carrier surface, and antimicrobial efficiency awaits further raising; (2) adhesion of metal ion and carrier a little less than, come off easily, service life is relatively poor.
The effect of nano material in medical science and biological study in recent years causes scientist's attention day by day, and wherein developing the nano-antibacterial product is an important developing direction.
Summary of the invention
Deficiency at prior art exists the object of the present invention is to provide the mesoporous carrying silver antimicrobials of a kind of novel nano;
Another object of the present invention is to provide the preparation method of this silver-carried antibacterial agent with nanometer porous.
The technical scheme that realizes objects of the present invention is as follows:
A kind of silver-carried antibacterial agent with nanometer porous is made up of carrier and silver, and specific surface area is 500～1500cm
3/ g, the aperture is 2～10nm, pore volume is 0.5～1.5cm
3/ g.
The active component of described mesoporous nano Ag-carried antibacterial is a simple substance silver, and carrier is the inorganic oxide with order mesoporous structure.
Described silver is selected from a kind of in silver nitrate or the silver ammino solution.
Described simple substance silver is 1.0～20% of silver-carried antibacterial agent with nanometer porous gross mass.
The carrier of described year silver is selected from silica, Al
2O
3, one or more the mixture in zeolite or the mesopore silicon oxide.
The preferred preferred meso pore silicon oxide material of silver-colored carrier that carries.
The preparation method of this silver-carried antibacterial agent with nanometer porous (is that mesopore silicon oxide is an example to carry silver-colored carrier) is:
A, polyethylene glycol-propane diols-polyethylene glycol triblock polymer (P123), water and HCl heated and stirred, temperature is controlled at 25～45 ℃, then add ethyl orthosilicate (TEOS) stirring reaction 12～48h, leave standstill then, suction filtration, washing obtain nanometer mesoporous silicon oxide SBA-15, removes surfactant through roasting at last;
B, get the said goods and add entry and ethanol (EtOH), splash into AgNO
3Solution behind ultrasonic 3～30min, in drying in oven, decomposes Ag behind dipping 12～48h then in the nitrogen of 300～500 ℃ of temperature and atmosphere of hydrogen, obtain silver-carried antibacterial agent with nanometer porous.
The solvent that adopts when introducing silver-colored antibacterial components is the second alcohol and water, and the two volume ratio is 1/0.5～1/10.
The nitrogen of described B step and the volume ratio of hydrogen are 5/1～15/1.
Because the size of general germ or bacterial cell is about about 50nm, therefore, the antibacterial agent that preparation has nano-scale can make activity enter cell interior mutually, realizes cell separation, and kill effectively and suppress virus and bacteria, have efficient, fast, the characteristics of lasting and broad-spectrum antiseptic.Secondly, the bulk effect of nano particle uniqueness can improve active distribution consistency degree mutually greatly with skin effect, increases its contact surface with germ or bacterium and amasss, thereby further improve germicidal efficiency; Utilize the quantum size effect of nano particle and macro quanta tunnel effect etc. can improve its electronics and level structure characteristic, improve sterilizing ability.In addition, nano particle has characteristics such as surface atom coordination degree of unsaturation height and The adsorbed hydroxyl content height, can be organic with majority and inorganic material (as textile, coating, leather, paper, printing ink, resin etc.) evenly mix, and produce stronger adsorption bond, not only adding the fashionable quality and the service life that can not influence product, and it is long-acting, high temperature resistant and not easy to change, have common antibacterial agent photostability and the heat endurance that can not compare, be particularly suitable for the health and the epidemic prevention demand of Public Goods and facility.
It is simple to operate that antibacterial agent of the present invention has the preparation method, do not produce environmental pollution in the preparation process, and Escherichia coli are had advantages such as very strong inhibition and kill activity.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of Ag-10-SBA-15-300.
Fig. 2 is the X-ray diffracting spectrum of Ag-10-MCM-41-300.
Fig. 3 is the TEM figure of Ag-10-SBA-15-300.
Fig. 4 is the TEM figure of Ag-10-MCM-41-300.
Embodiment
Further describe the present invention below in conjunction with accompanying drawing by specific embodiment and how to realize, enumerating these embodiment only is in order to set forth rather than limit by any way the present invention.
Embodiment 1
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mLTEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mLEtOH splash into 0.25g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 300 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-2.5-SBA-15-300.Be used at last for colibacillary antibacterial tests.
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mLTEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mLEtOH splash into 0.5gAgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 300 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-5-SBA-15-300.Be used at last for colibacillary antibacterial tests.
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mLTEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mLEtOH splash into 1g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 300 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-10-SBA-15-300.Be used at last for colibacillary antibacterial tests.
Embodiment 4
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mL TEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mL EtOH splash into 0.25g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 500 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-2.5-SBA-15-500.Be used at last for colibacillary antibacterial tests.
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mL TEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mL ethanol (EtOH) splash into 0.5g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 500 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-5-SBA-15-500.Be used at last for colibacillary antibacterial tests.
With 2g P123,15mL H
2O and 60mL 2M HCl add 4.47mLTEOS and stir 24h behind 35 ℃ of stirring 1h, leave standstill 24h then under 80 ℃ of conditions, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mLEtOH splash into 1g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 500 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/SBA-15 antibacterial agent, is labeled as Ag-10-SBA-15-500.Be used at last for colibacillary antibacterial tests.
With 0.8g hexadecyl trimethyl ammonium bromide (CTAB), 35g H
2O and 10g 1MNaOH continue to stir 48h add 4mL TEOS after stirring 1h under 40 ℃ of conditions after, obtain product through suction filtration, washing then, remove surfactant through 550 ℃ of roastings at last.Get 2g the said goods and add 20mL H
2O and 20mL EtOH splash into 1g AgNO
3(20%, m%) solution, behind the ultrasonic 3min, dipping spends the night the back in 80 ℃ of drying in oven, decomposes Ag then in 300 ℃ nitrogen and hydrogen (V/V=9/1) atmosphere, obtains the Ag/MCM-41 antibacterial agent, is labeled as Ag-10-MCM-41-300.
The foregoing description 1～7 is carried out antibacterial tests according to the antibiotic industry standard of Japan to Escherichia coli detect, obtain the minimal inhibitory concentration of each embodiment 1～7.List in table 1～table 3 respectively, each embodiment has all shown preferably for colibacillary antibacterial ability.The part-structure parameter of each antibacterial agent is listed in table 4.
The comparison of the minimal inhibitory concentration of the antibacterial agent of the Ag-SBA-15-300 of the different Ag load capacity of table 1
| sample | MIC(ppm) |
| Ag-2.5-SBA-15-300 Ag-5-SBA-15-300 Ag-10-SBA-15-300 | 300 200 90 |
The comparison of the antibacterial activity of each Ag-SBA-15 of the different sintering temperatures of table 2
| sample | MIC(ppm) |
| Ag-2.5-SBA-15-300 Ag-2.5-SBA-15-500 Ag-5-SBA-15-300 Ag-5-SBA-15-500 Ag-10-SBA-15-300 Ag-10-SBA-15-500 | 300 200 200 100 90 80 |
The comparison of the minimal inhibitory concentration of the Ag series antibacterial agent of table 3 different carriers
| sample | MIC(ppm) |
| Ag-10-SBA-15-300 Ag-10-MCM-41-300 | 90 100 |
The texture parameter of the Ag-SBA-15 antibacterial agent of the different Ag load capacity of table 4
| Sample | SBET(m 3/g) | D(nm) | V(cm 3/g) |
| Ag-2.5-SBA-15-300 Ag--5-SBA-15-300 Ag-10-SBA-15-300 Ag-2.5-SBA-15-500 Ag--5-SBA-15-500 Ag-10-SBA-15-500 | 671 682 640 504 627 602 | 5.27 5.28 3.80 5.29 5.29 5.82 | 1.04 1.06 0.78 0.80 0.99 1.16 |
Claims (9)
1, a kind of silver-carried antibacterial agent with nanometer porous is made up of carrier and silver, and specific surface area is 500～1500cm
3/ g, the aperture is 2～10nm, pore volume is 0.5～1.5cm
3/ g.
2, a kind of silver-carried antibacterial agent with nanometer porous according to claim 1 is characterized in that: the active component of described mesoporous nano Ag-carried antibacterial is a simple substance silver, and carrier is the inorganic oxide with order mesoporous structure.
3, a kind of silver-carried antibacterial agent with nanometer porous according to claim 1 is characterized in that: described silver is selected from a kind of in silver nitrate or the silver ammino solution.
4, according to claim 1,2 or 3 any described a kind of silver-carried antibacterial agent with nanometer porous, it is characterized in that: described simple substance silver is 1.0～20% of silver-carried antibacterial agent with nanometer porous gross mass.
5, according to claim 1 or 2 any described a kind of silver-carried antibacterial agent with nanometer porous, it is characterized in that: the carrier of described year silver is selected from silica, Al
2O
3, one or more the mixture in zeolite or the mesopore silicon oxide.
6, a kind of silver-carried antibacterial agent with nanometer porous according to claim 5 is characterized in that: the carrier that carries silver is selected from meso pore silicon oxide material.
7, according to the preparation method of claim 1,2,3,4,5 or 6 described a kind of silver-carried antibacterial agent with nanometer porous, the steps include:
A, with polyethylene glycol-propane diols-polyethylene glycol triblock polymer, water and HCl heating, temperature is controlled at 25～45 ℃, stir the back and add ethyl orthosilicate continuation stirring reaction 12～48h, leave standstill then, suction filtration, washing obtain nanometer mesoporous silicon oxide SBA-15, removes surfactant through roasting at last;
B, get the said goods and add entry and ethanol, splash into AgNO
3Solution behind ultrasonic 3～30min, in drying in oven, decomposes Ag behind dipping 12～48h then in the nitrogen of 300～500 ℃ of temperature and atmosphere of hydrogen, obtain silver-carried antibacterial agent with nanometer porous.
8, preparation method according to claim 7 is characterized in that: the solvent that adopts when introducing silver-colored antibacterial components is the second alcohol and water, and the two volume ratio is 1/0.5～1/10.
9, preparation method according to claim 7 is characterized in that: the nitrogen of described B step and the volume ratio of hydrogen are 5/1～15/1.
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