CN105772739A - Preparation method for graphene/nano-silver composite antibacterial material - Google Patents
Preparation method for graphene/nano-silver composite antibacterial material Download PDFInfo
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The invention provides a preparation method for a graphene/nano-silver composite antibacterial material and belongs to the technical field of new materials. The preparation method is characterized in that graphene oxide provided with silver ions in an adsorption manner is put into a reduction agent solution to be heated, the graphene/nano-silver composite material is obtained through centrifugal separation, and a reduction agent is glyoxylic acid. The method has the beneficial effects that reduction of the graphene oxide and the silver ions is sufficient, operation is simple, the process is controllable, and the obtained material has good antibacterial activity on common bacteria.
Description
Technical field
The invention belongs to field of new, the preparation method being specifically related to a kind of graphene/nano silver composite antibacterial material.
Background technology
Health is the topic that society people pay close attention to the most, but, in the environment of our life, there is substantial amounts of antibacterial, the health of the mankind in the growth and breeding serious threat of these antibacterials.Suitable antibacterial is selected to suppress the growth and breeding of noxious bacteria can effective guarantee people healthy.
Antibacterial can be divided into organic antibacterial agent, natural antibacterial agent, inorganic antiseptic according to structure difference.The antibacterial feature being respectively arranged with oneself of these three, organic antibacterial agent bactericidal effect is good, price is low, but poor stability, environmental pollution are serious.Natural antibacterial agent is from natural, and safety is high, environmental pollution is little, but thermostability, persistency are poor.Inorganic antiseptic has the good characteristics such as persistency is high, heat-resist, be not likely to produce drug resistance, safety is high, has wide development space and application potential in fields such as biological medicine, air cleaning, building coating, clothing, pottery, sanitary cooking utensils.In inorganic antiseptic field, most study surely belong to silver-series antibacterial agent, commercial inorganic antiseptic is silver-series antibacterial agent mostly at present.Silver-series antibacterial agent includes silver ion, argent and silver nano-grain.Compared with silver ion, argent, nano-Ag particles is due to the quantum effect of nanoparticle, small-size effect and great specific surface area so that the anti-microbial property of nano-Ag particles is far longer than traditional silver-series antibacterial agent.But, nano-Ag particles antibacterial exists that onset time is slow, poor stability, the deficiency such as easy to change, therefore, how to solve these problems, researches and develops efficient, nontoxic (low toxicity) and the lasting silver-series antibacterial agent of effect is the study hotspot of current Material Field.
Graphene is a kind of monolayer laminated structure two-dimensional material being made up of carbon atom, and its carbon atom is with sp2Hybrid orbital is formed has the cellular planar structure of hexangle type, has the excellent specific properties such as high-specific surface area, prominent mechanical property, heat conductivility and efficient electron transmission.Recent research indicate that: the layer structure of Graphene can directly pierce through the cell membrane of antibacterial, cause the leakage of antibacterial content and cause its death, and Graphene is less to mammiferous cytotoxicity.Additionally, Graphene as the excellent carrier of inorganic nano-particle, can make nanoparticle stability improve.Therefore, select suitable mode, prepare graphene/nano silver composite antibacterial material and not only can improve the stability of Nano silver grain, improve its water solublity, and both have synergetic antibacterial effect.
The preparation method of existing graphene/nano silver composite usually with graphene oxide and silver nitrate for raw material, is prepared by chemical reduction method, and hydrazine, sodium borohydride and hydroquinone are the reducing agents that redox graphene is the most frequently used.These reducing agents all have significantly high toxicity, and this brings very big risk to environment and human health.Therefore, the preparation method finding green, efficient, nontoxic new reducing agent and applicable commercial production Graphene thereof is urgently to be resolved hurrily.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of graphene/nano silver composite antibacterial material, the method selects the reduction of environment-friendly type reducing agent, it is to avoid the poisonous reducing agent injuries to environment such as hydrazine, sodium borohydride, hydroquinone.
The preparation method of a kind of graphene/nano silver composite antibacterial material provided by the invention, carries out as steps described below:
(1) by 2-4gNaNO3Add in 500mL four-hole boiling flask, add 100-150mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 10-20g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 35 ± 3 DEG C, react 100-180min；Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 200-250mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 10-20min, be subsequently adding the deionized water of 600-800mL by reaction terminating；Being simultaneously introduced 30-50mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black；Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 50-70 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 100-200mL deionized water, under the ultrasonic power of 300-500W, process 30-45min, under the speed of 8000-10000rpm, after centrifugal 5-8min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, add silver nitrate, obtain mixed solution；Evaporate mixed solution 10-18h at 60-100 DEG C, obtain the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion is put into the solution containing reducing agent carries out reduction treatment, obtain graphene/nano silver composite antibacterial material.
Wherein, the silver nitrate described in step (3) and graphite oxide mass ratio are: 0.01-0.5:1-2.
Wherein, the reducing agent described in step (4) is glyoxalic acid, and the concentration of reducing agent is 100-200g/L, and reducing agent and graphite oxide mass ratio are 10-20:1.
Wherein, reduction temperature 30-80 DEG C described in step (4), recovery time 4-8h.
The present invention adopts chemical method to prepare graphite oxide, and adopting eco-friendly glyoxalic acid is reducing agent, prepares graphene/nano silver composite antibacterial material, and preparation method is simple, reaction condition is gentle, controlled, is suitable for large-scale production.
Accompanying drawing explanation
The TEM figure of the graphene/nano silver anti-biotic material of Fig. 1 embodiment 1 preparation
XRD figure ((a) graphene oxide of the graphene/nano silver anti-biotic material of Fig. 2 embodiment 1 preparation；(b) graphene/silver composite material)
Raman spectrogram ((a) graphene oxide of the graphene/nano silver anti-biotic material of Fig. 3 embodiment 1 preparation；(b) graphene/silver composite material)
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiments present invention solely for the purpose of illustration, but not the scope being intended to limit the present invention in any manner.
Embodiment 1
(1) by 2gNaNO3Add in 500mL four-hole boiling flask, add 100mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 10g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 35 DEG C, react 100min.Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 200mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 10min, be subsequently adding the deionized water of 600mL by reaction terminating；Being simultaneously introduced 30mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black.Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 50 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 100mL deionized water, under the ultrasonic power of 300W, process 30min, under the speed of 8000rpm, after centrifugal 8min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, adding silver nitrate, silver nitrate and graphite oxide mass ratio is: 0.01:2；After mix homogeneously, evaporate mixed solution 18h at 60 DEG C, obtain the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion being put into 100mL mass concentration is carry out reduction treatment in 100g/L glyoxylic acid solution, and recovery time 8h at 30 DEG C obtains graphene/nano silver composite antibacterial material.
Embodiment 2
(1) by 4gNaNO3Add in 500mL four-hole boiling flask, add 150mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 20g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 32 DEG C, react 180min.Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 250mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 20min, be subsequently adding the deionized water of 800mL by reaction terminating；Being simultaneously introduced 50mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black.Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 70 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 200mL deionized water, under the ultrasonic power of 500W, process 45min, under the speed of 10000rpm, after centrifugal 5min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, adding silver nitrate, silver nitrate and graphite oxide mass ratio is: 0.5:1；After mix homogeneously, evaporate mixed solution 10h at 100 DEG C, obtain the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion being put into 100mL mass concentration is carry out reduction treatment in 200g/L glyoxylic acid solution, and recovery time 4h at 80 DEG C obtains graphene/nano silver composite antibacterial material.
Embodiment 3
(1) by 3gNaNO3Add in 500mL four-hole boiling flask, add 120mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 15g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 38 DEG C, react 120min.Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 220mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 15min, be subsequently adding the deionized water of 700mL by reaction terminating；Being simultaneously introduced 40mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black.Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 60 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 150mL deionized water, under the ultrasonic power of 400W, process 40min, under the speed of 9000rpm, after centrifugal 7min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, adding silver nitrate, silver nitrate and graphite oxide mass ratio is: 0.2:1.5, after mix homogeneously, evaporates mixed solution 12h at 80 DEG C, obtains the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion being put into 100mL mass concentration is carry out reduction treatment in 150g/L glyoxylic acid solution, and recovery time 6h at 60 DEG C obtains graphene/nano silver composite antibacterial material.
Embodiment 4
(1) by 2.5gNaNO3Add in 500mL four-hole boiling flask, add 130mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 12g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 34 DEG C, react 160min.Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 240mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 12min, be subsequently adding the deionized water of 750mL by reaction terminating；Being simultaneously introduced 35mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black.Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 55 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 180mL deionized water, under the ultrasonic power of 450W, process 35min, under the speed of 8500rpm, after centrifugal 6min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, adding silver nitrate, silver nitrate and graphite oxide mass ratio is: 0.1:1.5, evaporates mixed solution 16h at 70 DEG C, obtains the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion being put into 100mL mass concentration is carry out reduction treatment in 120g/L glyoxylic acid solution, and recovery time 7h at 50 DEG C obtains graphene/nano silver composite antibacterial material.
Embodiment 5
The antibiotic property test of sample is according to " GB/T21510-2008 nano inorganic material anti-microbial property detection method ", and strain selects escherichia coli and staphylococcus aureus.Test result is as shown in table 1:
Table 1 resulting materials bacteriostasis rate
Claims (4)
1. the preparation method of a graphene/nano silver composite antibacterial material, it is characterised in that: comprise the following steps:
(1) by 2-4gNaNO3Add in 500mL four-hole boiling flask, add 100-150mL98% concentrated sulphuric acid, cool down under condition of ice bath, when question response system temperature is lower than 5 DEG C, the 5g graphite powder dried is added under stirring condition, after mix homogeneously, it is stirred vigorously down, is slowly added to 10-20g potassium permanganate, reinforced process controls the temperature of reaction mixture less than 20 DEG C, after reinforced end, reacting liquid temperature is risen to 35 ± 3 DEG C, react 100-180min；Reacting liquid temperature is risen to 98 DEG C, is stirred vigorously down, be slowly added dropwise 200-250mL distilled water after terminating by reaction, after adding, controls reacting liquid temperature at about 98 DEG C, continues stirring 10-20min, be subsequently adding the deionized water of 600-800mL by reaction terminating；Being simultaneously introduced 30-50mL30% hydrogen peroxide and remove unreacted potassium permanganate, at this moment solution becomes vivid yellow from brownish black；Filtered while hot, and after washing away metal ion with 5% hydrochloric acid, with in deionized water wash to filtrate without SO4 2-(BaCl2Solution detects)；Then dry in the baking oven of 50-70 DEG C, it is thus achieved that graphite oxide powder；
(2) above-mentioned for 1g graphite oxide is joined in 100-200mL deionized water, under the ultrasonic power of 300-500W, process 30-45min, under the speed of 8000-10000rpm, after centrifugal 5-8min, disgorging, obtain graphene oxide dispersion；
(3) in the graphene oxide dispersion of step (2) gained, add silver nitrate, obtain mixed solution；Evaporate mixed solution 10-18h at 60-100 DEG C, obtain the graphene oxide of Adsorption For Ag ion；
(4) graphene oxide of above-mentioned Adsorption For Ag ion is put into the solution containing reducing agent carries out reduction treatment, obtain graphene/nano silver composite antibacterial material.
2. the preparation method of a kind of graphene/nano silver composite antibacterial material according to claim 1, it is characterised in that: described silver nitrate and graphite oxide mass ratio be: 0.01-0.5:1-2.
3. the preparation method of a kind of graphene/nano silver composite antibacterial material according to claim 1, it is characterised in that: described reducing agent is glyoxalic acid, and the concentration of reducing agent is 100-200g/L, and reducing agent and graphite oxide mass ratio are 10-20:1.
4. the preparation method of a kind of graphene/nano silver composite antibacterial material according to claim 1, it is characterised in that: described reduction temperature 30-80 DEG C, recovery time 4-8h.
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| CN106396386A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Photochromic health care ceramic and preparation method thereof |
| CN106887272A (en) * | 2017-03-16 | 2017-06-23 | 西安晶晟光电科技有限公司 | The preparation of chemical reduction method different-grain diameter graphene coated silver powder and the preparation method of slurry |
| CN107568246A (en) * | 2017-09-27 | 2018-01-12 | 郴州博太超细石墨股份有限公司 | A kind of Graphene antibiosis composite of loading nano silvery and preparation method thereof |
| CN107603480A (en) * | 2017-07-31 | 2018-01-19 | 常州建轩纺织品有限公司 | A kind of preparation method of Salt And Alkali Tolerance anticorrosion high polymer material |
| CN107815193A (en) * | 2017-11-17 | 2018-03-20 | 福建宸琦新材料科技有限公司 | Graphene-supported nano silver antimicrobials and graphene in-situ reducing loading nano silvery water anti-bacteria coating |
| CN107915221A (en) * | 2017-12-13 | 2018-04-17 | 天津宝兴威科技股份有限公司 | A kind of preparation method of the strong stannic oxide/graphene nano ag material of antibiotic property |
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| CN106396386B (en) * | 2016-08-29 | 2018-08-28 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of photochromic health-care ceramic and preparation method thereof |
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