CN113023720A - Preparation method of nitrated graphene oxide - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of nitrographene oxide, which comprises the steps of adding graphene oxide into deionized water to obtain a graphene oxide dispersion liquid with the concentration of 1-3 mg/mL, then adding concentrated nitric acid, stirring and mixing uniformly, carrying out hydrothermal reaction at 120-180 ℃ for 10-20 h, heating in a water bath and evaporating to dryness after the reaction is finished, and obtaining brown yellow powder, namely nitrographene oxide NGO. The preparation method of the nitrated graphene oxide is simple, good in water dispersion performance, high in oxidation degree, capable of remarkably improving the antibacterial performance of gram-positive bacteria and gram-negative bacteria, good in cell compatibility and capable of serving as a novel efficient antibacterial material to be used in the fields of biomedicine and the like.
Description
Technical Field
The invention belongs to the field of biomedical materials, and particularly relates to a preparation method of nitrated graphene oxide.
Background
Pathogenic bacteria are one of the biggest threats to human health, and can cause millions of people to infect each year. Since the discovery of penicillin in 1928, various antibiotics such as chloramphenicol, erythromycin, streptomycin, etc. have been discovered in succession and used medically to treat infections caused by various bacteria. However, with the extensive use of antibiotics, bacteria gradually change their own physiological or metabolic pathways to combat the effects of antibiotics and eventually evolve into resistant bacteria. Nowadays, with the continuous emergence, abuse and long-term use of various antibiotics, the drug resistance of various bacteria, especially pathogenic bacteria of animals, is continuously enhanced, even multidrug-resistant bacteria capable of resisting various antibiotics appear, thereby seriously threatening human health, and increasing medical cost and patient mortality. At present, about 70 million people die from drug-resistant bacterial infection every year in the world, and the number of people die from drug-resistant bacterial infection every year in the world is estimated to be more than 1000 thousands and far more than that of cancer death by 2050. Therefore, the defect of antibiotic resistance is overcome, a new non-antibiotic antibacterial material is developed, and the problem of bacterial resistance is solved. Although some common iodine-containing or chlorine-containing antibacterial agents have strong sterilization efficiency and can effectively overcome a bacterial drug resistance mechanism, the common iodine-containing or chlorine-containing antibacterial agents have toxic and side effects of skin allergy, metabolic disorder and the like in the practical application process, so that the common iodine-containing or chlorine-containing antibacterial agents are not suitable for treating wound infection of human bodies. The natural antibacterial agents such as chitosan, sodium alginate and the like have the advantages of safety, environmental protection and the like, but the thermal stability and the antibacterial aging performance are poor, so that the wide-range application of the antibacterial agents is restricted.
In recent years, inorganic metal antibacterial agents such as gold, silver, zinc, copper and the like and inorganic nano antibacterial materials represented by graphene have the advantages of good sterilization efficiency, small using amount, strong thermal stability, long antibacterial time, high biological safety and difficulty in generating drug resistance in the aspect of antibiosis due to specific sharp edges and large specific surface area, so that the antibacterial material has great application potential in the fields of biology, medical treatment, construction, environmental protection, clothing, medical appliances and the like.
Although researchers have made a lot of studies on the antibacterial properties of graphene, there are many controversies in the research results. Some researchers believe that the antibacterial activity of graphene is very weak, and some believe that graphene not only has no antibacterial activity, but also can improve bacterial adhesion to promote the formation and proliferation of bacterial biofilms. Therefore, the functional modification is fully utilized, so that the antibacterial fabric has good hydrophilicity, and meanwhile, the antibacterial performance of the antibacterial fabric can be effectively improved.
Disclosure of Invention
The invention aims to provide a preparation method of nitrated graphene oxide with good dispersibility and strong antibacterial ability.
Preparation of mono-nitro graphene oxide
The preparation method of the nitrated graphene oxide comprises the steps of adding Graphene Oxide (GO) into deionized water to obtain a graphene oxide dispersion liquid with the concentration of 1-3 mg/mL, adding concentrated nitric acid, stirring and mixing uniformly, carrying out hydrothermal reaction at 120-180 ℃ for 10-20 hours, heating in a water bath and drying by distillation after the reaction is finished, and obtaining brown yellow powder, namely the nitrated graphene oxide NGO. Wherein the graphene oxide is prepared by a traditional Hummers method; the volume ratio of the graphene oxide dispersion liquid to the concentrated nitric acid is 2: 1-9: 1; the mass concentration of the concentrated nitric acid is not less than 65 percent; stirring for 10-30 min; the temperature of the water bath is 60-80 ℃.
Structural characterization of NGO
1. FTIR analysis
The infrared spectra of GO and NGO are shown in figure 1. 3404 cm of GO-1The absorption peak is v O-H1734 cm in peak of stretching vibration-1The absorption peak is vC=O1630 cm-1Is vC=CCharacteristic absorption peak of 1400 cm-1Is vC-OH1051cm of-1Is vC-OCharacteristic absorption peak of (1). The results indicate that graphite has been successfully oxidized to GO. 1630 cm of GO after hydrothermal reaction-1V of (C)C=C、1400 cm-1V of (C)C-OHAnd 1051cm-1V ofC-OThe peak intensity is obviously reduced, which shows that part of oxygen-containing groups such as hydroxyl, epoxy and the like in GO and HNO3A reaction takes place. The reacted product NGO is 1569 cm-1、1384 cm-1、1250 cm-1And 868cm-14 new absorption peaks appear at the position, which respectively correspond to vNO2Antisymmetric and symmetric telescopic vibration and vC-NThe stretching vibration of (2). Wherein, 1384 cm-1And 1250 cm-1The absorption peak at (A) corresponds to C-NO2And O-NO2The telescopic vibration absorption band of (1). At the same time, 1400 cm in GO-1V of (C)C-OHIn NGO, the wave number is shifted to 1443cm-1This is due to-NO2The strong electron-withdrawing effect of the group. These results all demonstrate the presence of nitro groups in the NGO. In NGO at 1716 cm-1V. departmentC=OMay be due to concentrated HNO at high temperature3The oxidation effect on GO is enhanced, so that the oxidation degree is higher.
2. TEM analysis
TEM pictures of GO and NGO at different magnifications are shown in fig. 2 (a) and (b), respectively. The GO and the NGO are observed to have sharp and clear edges through a TEM (transmission electron microscope), a uniform plane lamellar structure is presented, and no obvious particles or impurities appear, so that the GO and the NGO samples prepared by the method are high in dispersity and cleanliness. While a distinct wrinkled structure is observed on the GO and NGO sheets, and the NGO becomes more interlamellar and more wrinkled, these wrinkles are caused by defects caused by the large number of oxygen-containing groups on the GO and NGO sheets, which upon intercalation into the middle of the graphite sheets result in a further increase in the interlamellar spacing of the NGO. These results all indicate that the degree of oxidation of the NGO is higher, consistent with the results obtained by FTIR, spectroscopy, and further explain the reason why the dispersion of NGO is significantly enhanced.
Three, NGO antibacterial property
Escherichia coli and staphylococcus aureus are used as model bacteria, and antibacterial properties of GO and NGO are researched. Treatment with GO and NGO at concentrations of 10 μ g/mL7The survival and growth of bacteria after 6 h in CFU/mL of E.coli and S.aureus is shown in FIG. 3. Compared with a control group without the antibacterial agent, the colony number on the agar plate is obviously reduced after the GO and the NGO are added, which shows that the GO and the NGO both have an inhibition effect on the growth of bacteria, and the results are consistent with the previous research on the antibacterial capacity of the GO. The colony count was observed to be minimal for the NGO treated group and significantly less than for the GO treated and control groups, with NGO exhibiting greater antimicrobial performance than GO at the same concentration. According to statistics, under the same concentration (30 mu g/mL), the sterilization rates of GO and NGO on Escherichia coli are respectively21.36 percent and 91.26 percent, the sterilization rate to staphylococcus aureus is 16.42 percent and 83.07 percent respectively, which indicates that the staphylococcus aureus is subjected to concentrated HNO3The antibacterial performance of the hydrothermally modified NGO is stronger than that of GO, and the antibacterial capability to escherichia coli and staphylococcus aureus is improved by about 4 times than that of GO.
In conclusion, the GO is used as a raw material, a large number of oxygen-containing functional groups such as carboxyl, hydroxyl and epoxy groups on the surface and the edge of the GO are utilized, the GO is subjected to nitromodification by concentrated nitric acid, so that the oxidation degree of the GO is higher, the dispersibility of the GO is better, and the bactericidal capacity is enhanced by improving the physical cutting and oxidative stress effect in the contact process of the GO and bacteria. The nitrated graphene oxide derivative (NGO) has good dispersibility, strong antibacterial ability and low cytotoxicity, and can be used as a novel efficient antibacterial material in the fields of biomedicine and the like.
Drawings
FIG. 1 is an infrared spectrum of GO and NGO;
FIG. 2 is a transmission electron microscope picture of GO and NGO;
fig. 3 is a comparison of antibacterial performance of GO and NGO.
Detailed Description
The preparation method of the nitrated graphene oxide of the present invention is further described below by specific examples.
Example 1
(1) Preparation of GO
Taking 24 mL of concentrated H2SO4 Adding 100 mL beaker, heating in oil bath to 80 deg.C, and sequentially adding K2S2O8And P2O55g of each, stirring evenly, adding 6g of graphite powder, and pre-oxidizing for 4.5 h. And after the reaction is finished, adding 1000 mL of deionized water into the mixture, standing for 12 h, discarding the supernatant, performing suction filtration on the precipitate until the precipitate is dried, and drying at 60 ℃ for 24 h for later use.
② adding 240 mL of cold concentrated H into the dried graphite powder after preoxidation2SO4 Adding KMnO after stirring uniformly430 g of powder, placing a beaker in an ice-water bath, and keeping the temperature of a reaction system in the step below 20 ℃ to KMnO4And completely dissolving.
③ will mixAfter the temperature of the combined system is raised to 35 ℃, stirring and reacting for 2 h, and continuously adding 500 mL of deionized water into the reaction system, stirring and reacting for 2 h. Then 1.4L of deionized water and 40 mL of 30% H were added2O2A brownish yellow aqueous solution was obtained.
And fourthly, washing the brown yellow aqueous solution with 500 mL of 5% HCl and 500 mL of deionized water respectively, and standing for 12 hours. Discarding part of the supernatant, diluting to a certain concentration, dialyzing with deionized water until BaCl is used2No precipitation was observed by titration of the solution. And carrying out ultrasonic treatment on the dialyzed brown aqueous solution for 2 hours to obtain a stably dispersed GO aqueous solution.
(2) Preparation of Nitrated Graphene Oxide (NGO)
Firstly, adding the GO into deionized water to obtain a dispersion liquid with the concentration of 1-3 mg/mLGO;
secondly, taking 90mL of 1 mg/mL GO, adding 10 mL of concentrated nitric acid (wt is more than or equal to 65%) while stirring lightly, and continuously stirring for 10-30 min to fully and uniformly mix the GO with the concentrated nitric acid;
thirdly, transferring the reaction liquid into a 100 mL high-pressure reaction kettle with a stainless steel Teflon lining, and carrying out closed reaction for 10 hours at the high temperature of 120 ℃;
and fourthly, after the reaction is finished, transferring the cooled reaction solution to a 250 mL beaker, heating in a water bath at the temperature of 60-80 ℃ and evaporating to dryness to obtain brown yellow powder, namely NGO. Example adjustment of specific data for different important control conditions, and inappropriate requests
Bactericidal performance of NGO: NGO at a concentration of 30. mu.g/mL against E.coli (10)7CFU/mL) of the specimen, and the sterilization rate of the specimen against Staphylococcus aureus (10)7CFU/mL) was 51.36%.
Example 2
(1) Preparation of GO: the same as example 1;
(2) preparation of Nitrated Graphene Oxide (NGO)
Firstly, adding the GO into deionized water to obtain a dispersion liquid with the concentration of 1-3 mg/mLGO;
secondly, taking 80 mL of GO with the concentration of 2 mg/mL, adding 20mL of concentrated nitric acid (wt is more than or equal to 65%) while stirring lightly, and continuously stirring for 10-30 min to fully and uniformly mix;
thirdly, transferring the reaction liquid into a 100 mL high-pressure reaction kettle with a stainless steel Teflon lining, and carrying out closed reaction for 20 hours at the high temperature of 150 ℃;
and fourthly, after the reaction is finished, transferring the cooled reaction solution to a 250 mL beaker, heating in a water bath at the temperature of 60-80 ℃ and evaporating to dryness to obtain brown yellow powder, namely NGO.
Bactericidal performance of NGO: NGO at a concentration of 30. mu.g/mL against E.coli (10)7CFU/mL) of the bacteria at a ratio of 91.26% against Staphylococcus aureus (10)7CFU/mL) was 83.07%.
Example 3
(1) Preparation of GO: the same as example 1;
(2) preparation of Nitrated Graphene Oxide (NGO)
Firstly, adding the GO into deionized water to obtain a dispersion liquid with the concentration of 1-3 mg/mLGO;
secondly, taking 70 mL of GO with the concentration of 3mg/mL, adding 30mL of concentrated nitric acid (wt is more than or equal to 65%) while stirring lightly, and continuously stirring for 10-30 min to fully and uniformly mix;
thirdly, transferring the reaction liquid into a 100 mL high-pressure reaction kettle with a stainless steel Teflon lining, and carrying out closed reaction for 15h at the high temperature of 180 ℃;
and fourthly, after the reaction is finished, transferring the cooled reaction solution to a 250 mL beaker, heating in a water bath at the temperature of 60-80 ℃ and evaporating to dryness to obtain brown yellow powder, namely NGO.
Bactericidal performance of NGO: NGO at a concentration of 30. mu.g/mL against E.coli (10)7CFU/mL) of the bacteria at a ratio of 85.32% against Staphylococcus aureus (10)7CFU/mL) was 70.81%.
Claims (6)
1. A preparation method of nitrographene oxide comprises the steps of adding graphene oxide into deionized water to obtain a graphene oxide dispersion liquid with the concentration of 1-3 mg/mL, then adding concentrated nitric acid, stirring and mixing uniformly, carrying out hydrothermal reaction at 120-180 ℃ for 10-20 hours, and after the reaction is finished, heating in a water bath and drying by distillation to obtain brown yellow powder, namely nitrographene oxide NGO.
2. The method for preparing the nitrated graphene oxide according to claim 1, which is characterized in that: the graphene oxide is prepared by a traditional Hummers method.
3. The preparation method of the regenerative bacterial cellulose composite hydrogel dressing as claimed in claim 1, wherein the preparation method comprises the following steps: the volume ratio of the graphene oxide dispersion liquid to the concentrated nitric acid is 2: 1-9: 1.
4. The preparation method of the regenerative bacterial cellulose composite hydrogel dressing as claimed in claim 1, wherein the preparation method comprises the following steps: the mass concentration of the concentrated nitric acid is not less than 65%.
5. The preparation method of the regenerative bacterial cellulose composite hydrogel dressing as claimed in claim 1, wherein the preparation method comprises the following steps: the stirring time is 10-30 min.
6. The preparation method of the regenerative bacterial cellulose composite hydrogel dressing as claimed in claim 1, wherein the preparation method comprises the following steps: the temperature of the water bath is 60-80 ℃.
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