CN108584959A - A kind of preparation method for being layered two-dimentional transition metal carbide or the carbonization Tritanium/Trititanium of carbonitride-two improving antibiotic property - Google Patents
A kind of preparation method for being layered two-dimentional transition metal carbide or the carbonization Tritanium/Trititanium of carbonitride-two improving antibiotic property Download PDFInfo
- Publication number
- CN108584959A CN108584959A CN201810420678.3A CN201810420678A CN108584959A CN 108584959 A CN108584959 A CN 108584959A CN 201810420678 A CN201810420678 A CN 201810420678A CN 108584959 A CN108584959 A CN 108584959A
- Authority
- CN
- China
- Prior art keywords
- mxene
- layering
- preparation
- antibiotic property
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention discloses a kind of layering MXene Ti improving antibiotic property3C2Preparation method, include the following steps：(1) by Ti3AlC2MAX phase ceramics powder and the mixing of HF solution, obtained mixed liquor are stirred to react under the conditions of oil bath, obtain intermediate solution after reaction；(2) intermediate solution is subjected to washing centrifugation using deionized water, until pH=5~6 of supernatant；Continue wash centrifuging with ethyl alcohol to obtain sediment, is dried later, obtains MXene Ti3C2Powder；(3) the MXene Ti that will be obtained in step (2)3C2Powder is sufficiently mixed stirring with hydrazine hydrate or isopropyl amine aqueous solution, and intermediate solution is obtained after being stirred to react；(4) intermediate solution obtained in step (3) is ultrasonically treated, the solution membrane filtration being ultrasonically treated after terminating is improved the layering MXene Ti of antibiotic property after dry3C2.The layering MXene Ti for improving antibiotic property3C2Preparation method can realize MXene Ti3C2Preparation and layering, and layering MXene Ti obtained3C2Antibiotic property with raising.
Description
Technical field
The present invention relates to MXene-Ti3C2Preparation field, and in particular to it is a kind of improve antibiotic property layering MXene-
Ti3C2Preparation method.
Background technology
With the rapid development of nano material, more and more nano materials are found to study and are applied to every field
In, including Medical Devices, water process, in the application of the field of public health such as food packaging and textile industry, antimicrobial nano
Material has obtained extensive research.After graphene in 2004 is successfully synthesized, since the good physical chemistry that it has is special
Property, thus significant progress is obtained in every field, and it is higher and higher for its application requirement.Existing research table
Bright, graphene has certain antibiotic property, therefore has started the research boom to two-dimensional nano anti-biotic material.
MXene-Ti3C2As a kind of novel two-dimentional transition metal carbide, it has similar lamella knot with graphene
Structure has good physicochemical characteristics.More some researches show that, antibacterial abilities to be higher than graphene and Graphene derivative,
Biomedical sector has a good application prospect.
Its preparation and layering and application is being extensively studied, MXene-Ti3C2It is typically to use chemical etching method
From MAX phases (Ti3AlC2) in Al is stripped out to obtain, common etching agent has HF, NH4HF2And HCl's and LiF is mixed
Close liquid.The MXene-Ti of single lamella can not be obtained by the method for chemical etching3C2, also need to be layered by ultrasonic wave added
Mode be allowed to remove layer by layer.
Currently, selecting HF as etching agent mostly, then react under the conditions of magnetic agitation.Point with antibiotic property
Layer MXene-Ti3C2Preparation method is mainly with the MXene-Ti prepared3C2Material with water or dimethyl sulfoxide (DMSO)
(DMSO) it is ultrasonically treated under the conditions of argon gas after disperseing.But with the MXene-Ti of layering prepared by both methods3C2Layering
Effect is not satisfactory, and antibiotic property is not also high, limits its further development as anti-biotic material.
The patent document of Publication No. CN107324335A discloses a kind of MXene- preparing layering using ultrasonic wave added
Ti3C2Method, include the following steps：1) by Ti3AlC2- MAX phase ceramics powder and the mixing of HF solution, are then added dimethyl
Sulfoxide obtains mixed liquor；2) mixed liquor is ultrasonically treated, after the completion of ultrasound, is then stirred to react under the conditions of oil bath；Institute
It states supersound process and is stirred to react and be alternately repeated progress, obtain intermediate solution after reaction；3) by intermediate solution using go from
Sub- water carries out washing centrifugation, until the pH=5-6 of supernatant；Continue wash centrifuging with ethyl alcohol to obtain sediment, Zhi Hougan
Dry processing, the MXene-Ti being layered3C2.This method can be achieved at the same time MXene-Ti3C2Preparation and layering.
Invention content
The purpose of the present invention is to provide a kind of a kind of layering two dimension transition improving antibiotic property of the layering improving antibiotic property
Metal carbides or the carbonization Tritanium/Trititanium of carbonitride-two (MXene-Ti3C2) preparation method.The layering for improving antibiotic property
MXene-Ti3C2Preparation method can realize MXene-Ti3C2Preparation and layering, and layering MXene-Ti obtained3C2
Improve its antibiotic property.
Technical solution provided by the invention is：
A kind of layering MXene-Ti improving antibiotic property3C2Preparation method, include the following steps：
(1) by Ti3AlC2- MAX phase ceramics powder and the mixing of HF solution, obtained mixed liquor stir anti-under the conditions of oil bath
It answers, obtains intermediate solution after reaction；
(2) intermediate solution is subjected to washing centrifugation using deionized water, until pH=5~6 of supernatant；Continue to use ethyl alcohol
It carries out washing centrifugation and obtains sediment, be dried later, obtain MXene-Ti3C2Powder；
(3) MXene-Ti that will be obtained in step (2)3C2The solution of powder and hydrazine hydrate or isopropylamine is sufficiently mixed stirring,
Intermediate solution is obtained after being stirred to react；
(4) intermediate solution obtained in step (3) is ultrasonically treated, the solution filter membrane being ultrasonically treated after terminating
Filtering is improved the layering MXene-Ti of antibiotic property after dry3C2。
The mass concentration of HF solution is 40~49% in the step (1).
The mass concentration of HF solution can lead to Ti less than the lower limit of above range3AlC2- MAX phase ceramics powder is not exclusively carved
Erosion, it is excessively high higher than upper limit HF solution concentrations that reaction can be caused excessively violent.
Ti in the step (1)3AlC2The rate of charge of-MAX phase ceramics powder and HF solution is 1g:16~24ml.
Ti3AlC2- MAX phase ceramics powder can cause to react incomplete less than lower limit with the rate of charge of HF solution, be higher than the upper limit
HF is excessive then uneconomical.
The temperature being stirred to react in the step (1) is 40~60 DEG C, and the time being stirred to react is 24~36h.
The range of the above-mentioned temperature and time being stirred to react ensure that the reaction was complete.
The rotating speed of washing centrifugation is 2500~3500rpm in the step (2).
The rotating speed of washing centrifugation can cause to precipitate incomplete waste of material less than lower limit, complete higher than upper limit precipitation, turn
Speed increases then meaningless.
MXene-Ti in the step (3)3C2The rate of charge of powder and hydrazine hydrate is 1g:80~120ml.
MXene-Ti3C2Powder can cause to react incomplete less than the lower limit of above range with the rate of charge of hydrazine hydrate, be higher than
Upper limit hydrazine hydrate is excessive then uneconomical.
MXene-Ti in the step (3)3C2The rate of charge of powder and isopropyl amine aqueous solution is 1g：80~120ml, it is described
The volumetric concentration of isopropyl amine aqueous solution is 15~25%.
MXene-Ti3C2Powder can cause to react incomplete less than the lower limit of above range with the rate of charge of isopropylamine, be higher than
Upper limit isopropylamine is excessive then uneconomical.
MXene-Ti in the step (3)3C2Powder is mixed with hydrazine hydrate, the layering MXene- that step (4) obtains
Ti3C2Lattice constant beInterlamellar spacing isLamellar spacing is 21-27nm.
MXene-Ti in the step (3)3C2Powder is mixed with isopropylamine, the layering MXene- that step (4) obtains
Ti3C2Lattice constant beInterlamellar spacing isLamellar spacing is 10-17nm.
Further, MXene-Ti in the step (3)3C2Powder is mixed with hydrazine hydrate, the layering that step (4) obtains
MXene-Ti3C2Lattice constant beInterlamellar spacing isLamellar spacing is 21.8-
27.6nm。
Further, MXene-Ti in the step (3)3C2Powder is mixed with isopropylamine, the layering that step (4) obtains
MXene-Ti3C2Lattice constant beInterlamellar spacing isLamellar spacing is 10.6-
17nm。
The temperature being stirred to react in the step (3) is 20~25 DEG C, and the time being stirred to react is 16~18h.
The range of the above-mentioned temperature and time being stirred to react ensure that the reaction was complete and the safety of reaction.
The frequency being ultrasonically treated in the step (4) is 40~50kHz, and the power of supersound process is 80~100%.
The frequency of supersound process can cause layering incomplete less than lower limit, lamella can be caused broken higher than the upper limit.
The layering of the power assurance of above-mentioned supersound process is complete.
Further, the mass concentration of HF solution is 49%, Ti in the step (1)3AlC2- MAX phase ceramics powder with
The rate of charge of HF solution is 5g:100ml；The temperature being stirred to react in the step (2) is 50 DEG C, and the time being stirred to react is
The rotating speed that 36h, washing centrifuge is 3500rpm；MXene-Ti in the step (3)3C2Powder and hydrazine hydrate or isopropyl amine aqueous solution
Rate of charge be 1g:100ml, the volumetric concentration of the isopropyl amine aqueous solution is 25%, the temperature that is stirred to react is 25 DEG C；The step
Suddenly the frequency being ultrasonically treated in (4) is 45kHz.Layering MXene-Ti prepared by above range3C2With more suitable interlayer
It is more preferable away from, lattice constant and lamellar spacing, anti-microbial property.
Compared with the existing technology, beneficial effects of the present invention are embodied in：
(1) present invention is inserted into MXene-Ti using hydrazine hydrate or isopropylamine3C2Interlayer, MXene- can be significantly increased
Ti3C2Interlamellar spacing, after be allowed to remove layer by layer by way of supersound process, layered effect is good.
(2) layering MXene-Ti provided by the invention3C2For two-dimensional layer material, antibiotic property is improved, antibiotic property is better than biography
System two-dimension nano materials graphene, has further widened two-dimensional layer MXene-Ti3C2The application field of material.
Description of the drawings
Fig. 1 is layering MXene-Ti prepared by embodiment 1-2 and comparative example 1-23C2Be not layered MXene-Ti3C2's
XRD；
Fig. 2 is not to be layered MXene-Ti3C2Transmission electron microscope picture；
Fig. 3 is layering MXene-Ti prepared by embodiment 13C2Transmission electron microscope picture；
Fig. 4 is layering MXene-Ti prepared by embodiment 23C2Transmission electron microscope picture；
Fig. 5 is layering MXene-Ti prepared by embodiment 1-2 and comparative example 1-23C2Be not layered MXene-Ti3C2Not
With the cell inactivation rate under the time；
Fig. 6 is layering MXene-Ti prepared by embodiment 1-2 and comparative example 1-23C2Be not layered MXene-Ti3C2Not
With the cell inactivation rate under concentration；
Fig. 7 is the fluorescent staining figure of normal bacterial cells；
Fig. 8 is the fluorescent staining figure of apoptotic bacteria cell；
Fig. 9 is layering MXene-Ti prepared by embodiment 13C2With the fluorescent staining figure after bacterial cell co-incubation；
Figure 10 is layering MXene-Ti prepared by embodiment 23C2With the fluorescent staining figure after bacterial cell co-incubation；
Figure 11 is layering MXene-Ti prepared by comparative example 13C2With the fluorescent staining figure after bacterial cell co-incubation；
Figure 12 is layering MXene-Ti prepared by comparative example 23C2With the fluorescent staining figure after bacterial cell co-incubation.
Specific implementation mode
Below in conjunction with the accompanying drawings, present invention is further described in detail for embodiment and comparative example.
Embodiment 1
(1)5g Ti3AlC2- MAX phase ceramics powder is slowly added into the HF solution that 100mL mass concentrations are 49%,
Obtain intermediate solution；
(2) intermediate solution that step (1) obtains is reacted into 36h in magnetic stirring apparatus under the conditions of 50 DEG C of oil bath；
(3) after reaction, acquired solution is divided evenly into 6 parts to pour into the centrifugal bottle of 6 350mL, adds distilled water
To at 2/3, concussion centrifuges 5min after shaking up under the rotating speed of 3500rpm, pours out supernatant after taking supernatant to survey pH value, and spend
Ionized water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 6 times；The pH=5.6 of last supernatant is measured,
Absolute ethyl alcohol washing precipitate is used again, is centrifuged after concussion, identical rotating speed and centrifugation time is kept to be repeated twice；
(4) it is filtered under diminished pressure after obtained precipitation being completely dispersed suspension with absolute ethyl alcohol, it is dry that obtained powder is put into vacuum
It is dried 24 hours under room temperature in dry case, obtains MXene-Ti3C2Powder；
(5) MXene-Ti that will be obtained in 1g steps (4)3C2Powder is dispersed in 100ml hydrazine hydrates (HMH), in magnetic
In power blender 18h is stirred to react at 25 DEG C；
(6) after reaction, throw aside supernatant after acquired solution being centrifuged 15min under the rotating speed of 3500rpm, spend from
Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 2 times；
(7) obtained sediment is dispersed in 500ml deionized waters, is ultrasonically treated under the conditions of argon gas
(power is 100% and frequency is 45k Hz) 6h；
(8) solution after supersound process is uniformly poured into surface plate, the vacuum under room temperature in vacuum drying chamber
Drying for 24 hours, is improved the layering MXene-Ti of antibiotic property3C2Material.
The layering MXene-Ti of preparation3C2The XRD spectra of material is not as shown in Figure 1, with MXene-Ti is layered3C2XRD
Spectrogram is compared, and after the layered shaping of hydrazine hydrate, the low angle in XRD diagram produces apparent displacement；The layering of preparation
MXene-Ti3C2The interlamellar spacing and lattice constant of material are as shown in table 1, and are not layered MXene-Ti3C2Interlamellar spacing and lattice it is normal
Number is compared, and interlamellar spacing and lattice constant significantly increase, and show that layered shaping has further been unlocked and are not layered MXene-Ti3C2's
Layer structure, and there is quite high efficiency.
The layering MXene-Ti of preparation3C2The transmission electron microscope picture of material with Fig. 2 as shown in figure 3, be not layered MXene-
Ti3C2Transmission electron microscope picture compare, after the layered shaping of hydrazine hydrate, the layering MXene-Ti of single layer or few layer3C2
Laminated structure is in the majority, and translucent tablet is shown as in figure, may determine that its thickness by the depth of color.
The layering MXene-Ti of preparation3C2The anti-microbial property of material is as shown in Figure 5 and Figure 6, by the MXene-Ti of layering3C2
It is dispersed in the mother liquor for being configured to 2mg/ml in deionized water, Escherichia coli are exposed to the layering MXene- of various concentration
Ti3C2The middle culture different time.It takes the bacterium solution after culture to carry out being serially diluted tablet numeration, calculates the mistake of Bacillus coli cells
Motility rate, as a result as shown in Figure 5 and Figure 6, it can be seen from the figure that the MXene- by the obtained layering of hydrazine hydrate layered shaping
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 90% or more within exposure 3h, reaches 98% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than.
The layering MXene-Ti of preparation3C2With progress bacterial cell fluorescent staining, fluorescent staining figure after bacterium co-incubation 3h
As shown in figure 9, wherein Fig. 7 is the fluorescent staining figure of normal bacterial cells, Fig. 8 is the fluorescent staining figure of apoptotic bacteria cell.From
In Fig. 7-9 it can be seen that after exposure 3h, much larger than normal bacterial cells, (arrow meaning is just to apoptotic bacteria cell proportion
Normal bacterial cell), illustrate the obtained layering MXene-Ti after hydrazine hydrate layered shaping3C2With stronger bactericidal effect.
Embodiment 2
MXene-Ti3C2Powder preparation method is in the same manner as in Example 1.
(1) by 1g MXene-Ti3C2It is water-soluble that powder is dispersed in the isopropylamine (IPA) that 100ml volumetric concentrations are 25%
In liquid, 18h is stirred to react at 25 DEG C in magnetic stirring apparatus；
(2) after reaction, throw aside supernatant after acquired solution being centrifuged 15min under the rotating speed of 3500rpm, spend from
Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 2 times；
(3) obtained sediment is dispersed in 500ml deionized waters, is ultrasonically treated under the conditions of argon gas
(power is 100% and frequency is 45k Hz) 6h；
(4) solution after supersound process is uniformly poured into surface plate, the vacuum under room temperature in vacuum drying chamber
Drying for 24 hours, is improved the layering MXene-Ti of antibiotic property3C2Material
The layering MXene-Ti of preparation3C2The XRD spectra of material is not as shown in Figure 1, with MXene-Ti is layered3C2XRD
Spectrogram is compared, and after the layered shaping of isopropylamine, the low angle in XRD diagram produces apparent displacement；The layering of preparation
MXene-Ti3C2The interlamellar spacing and lattice constant of material are as shown in table 1, and are not layered MXene-Ti3C2Interlamellar spacing and lattice it is normal
Number is compared, and interlamellar spacing and lattice constant significantly increase, and show that layered shaping has further been unlocked and are not layered MXene-Ti3C2's
Layer structure, and there is quite high efficiency.
The layering MXene-Ti of preparation3C2The transmission electron microscope picture of material with Fig. 2 as shown in figure 4, be not layered MXene-
Ti3C2Transmission electron microscope picture compare, after the layered shaping of isopropylamine, the layering MXene-Ti of single layer or few layer3C2
Laminated structure is in the majority, shows as translucent tablet in Fig. 4, may determine that its thickness by the depth of color.
The layering MXene-Ti of preparation3C2The anti-microbial property of material is as shown in Figure 5 and Figure 6, by the MXene-Ti of layering3C2
It is dispersed in the mother liquor for being configured to 2mg/ml in deionized water, Escherichia coli are exposed to the layering MXene- of various concentration
Ti3C2The middle culture different time.It takes the bacterium solution after culture to carry out being serially diluted tablet numeration, calculates the mistake of Bacillus coli cells
Motility rate, as a result as shown in Figure 5 and Figure 6, it can be seen from the figure that the MXene- by the obtained layering of isopropylamine layered shaping
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 90% or more within exposure 3h, reaches 95% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than.
The layering MXene-Ti of preparation3C2With progress bacterial cell fluorescent staining, fluorescent staining figure after bacterium co-incubation 3h
As shown in Figure 10, wherein Fig. 7 is the fluorescent staining figure of bacterial cell, and Fig. 8 is the fluorescent staining figure of normal cell.From Fig. 7-8 and
In Figure 10 it can be seen that after exposure 3h, much larger than normal cell, (arrow meaning is normal thin to apoptotic bacteria cell proportion
Bacterium cell), illustrate the obtained layering MXene-Ti after isopropylamine layered shaping3C2With stronger bactericidal effect.
Embodiment 3
The layering MXene-Ti provided such as embodiment 13C2, difference is, 80 mL mass concentrations are added in step (1) and are
49% HF solution, the temperature being stirred to react in the step (1) are 40 DEG C, and the time being stirred to react is 36h, the step
(2) rotating speed of washing centrifugation is 2500rpm in, and the temperature being stirred to react in the step (3) is 20 DEG C, the time being stirred to react
For 18h, the frequency being ultrasonically treated in the step (4) is 40kHz, and the power of supersound process is 100%, will in step (5)
MXene-Ti3C2Powder is dispersed in 80ml hydrazine hydrates.
The layering MXene-Ti of preparation3C2The interlamellar spacing and lattice constant of material are as shown in table 2；The MXene- of layering
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 87% or more within exposure 3h, reaches 93% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than；The layering MXene-Ti of preparation3C2It withers after exposure 3h with progress bacterial cell fluorescent staining after bacterium co-incubation 3h
Bacterial cell proportion is died more slightly to reduce.
Embodiment 4
The layering MXene-Ti provided such as embodiment 13C2, difference is, 120 mL mass concentrations are added in step (1)
For 40% HF solution, the temperature being stirred to react in the step (1) is 60 DEG C, and the time being stirred to react is the step for 24 hours
(2) rotating speed of washing centrifugation is 3000rpm in, and the temperature being stirred to react in the step (3) is 25 DEG C, the time being stirred to react
For 16h, the frequency being ultrasonically treated in the step (4) is 50kHz, and the power of supersound process is 80%, will in step (5)
MXene-Ti3C2Powder is dispersed in 120ml hydrazine hydrates.
The layering MXene-Ti of preparation3C2The interlamellar spacing and lattice constant of material are as shown in table 1；The MXene- of layering
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 89% or more within exposure 3h, reaches 96% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than；The layering MXene-Ti of preparation3C2It withers after exposure 3h with progress bacterial cell fluorescent staining after bacterium co-incubation 3h
Bacterial cell proportion is died more slightly to reduce.
Embodiment 5
The layering MXene-Ti provided such as embodiment 13C2, difference is, by 1g MXene- in the step (1)
Ti3C2Powder is dispersed in isopropylamine (IPA) aqueous solution that 120ml volumetric concentrations are 15%.
The layering MXene-Ti of preparation3C2The interlamellar spacing and lattice constant of material are as shown in table 1；The MXene- of layering
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 88% or more within exposure 3h, reaches 94% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than；The layering MXene-Ti of preparation3C2It withers after exposure 3h with progress bacterial cell fluorescent staining after bacterium co-incubation 3h
Bacterial cell proportion is died more slightly to reduce.
Embodiment 6
The layering MXene-Ti provided such as embodiment 13C2, difference is, by 1g MXene- in the step (1)
Ti3C2Powder is dispersed in isopropylamine (IPA) aqueous solution that 80ml volumetric concentrations are 25%.
The layering MXene-Ti of preparation3C2The interlamellar spacing and lattice constant of material are as shown in table 1；The MXene- of layering
Ti3C2Antibiotic property be significantly higher than and be not layered MXene-Ti3C2, and the dependence of time and concentration is presented, bacterial cell exists
Inactivation rate reaches 92% or more within exposure 3h, reaches 96% to the activity suppression of bacterial cell in a concentration of 100ug/mL
More than；The layering MXene-Ti of preparation3C2It withers after exposure 3h with progress bacterial cell fluorescent staining after bacterium co-incubation 3h
Bacterial cell proportion is died compared with embodiment 2 compared to slightly reduction.
Comparative example 1
(1) by 1g MXene-Ti3C2Powder is dispersed in 100ml deionized waters, in magnetic stirring apparatus at 25 DEG C
Stir 18h；
(2) after reaction, throw aside supernatant after acquired solution being centrifuged 15min under the rotating speed of 3500rpm, spend from
Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 2 times；
(3) obtained sediment is dispersed in 500ml deionized waters, is ultrasonically treated under the conditions of argon gas
(power is 100% and frequency is 45k Hz) 6h；
(4) solution after supersound process is uniformly poured into surface plate, the vacuum under room temperature in vacuum drying chamber
It dries for 24 hours, obtained layering MXene-Ti3C2Material.
The layering MXene-Ti of preparation3C2The XRD spectra of material is not as shown in Figure 1, with MXene-Ti is layered3C2XRD
Spectrogram is compared, the layering MXene-Ti of preparation3C2Material does not generate apparent displacement；The layering MXene-Ti of preparation3C2Material
Interlamellar spacing and lattice constant are as shown in table 1, and are not layered MXene-Ti3C2Interlamellar spacing and lattice constant compare, it is only only light
Micro- increase shows that certain lamination is played in ultrasonication, but inefficient.
The layering MXene-Ti of preparation3C2The anti-microbial property of material is as shown in Figure 5 and Figure 6, by the MXene-Ti of layering3C2
It is dispersed in the mother liquor for being configured to 2mg/ml in deionized water, Escherichia coli are exposed to the layering MXene- of various concentration
Ti3C2The middle culture different time.It takes the bacterium solution after culture to carry out being serially diluted tablet numeration, calculates the mistake of Bacillus coli cells
Motility rate, as a result as shown in Figure 5 and Figure 6, prepared layering MXene-Ti3C2Material has certain antibiotic property, and antibiotic property
Time-and concentration-dependent is presented, but antibiotic property is significantly lower than the layering MXene-Ti that isopropylamine or hydrazine hydrate are layered3C2Material
Material, cell inactivation rate after exposure 5h can be only achieved 90%, when concentration reaches 200ug/mL only to the activity suppression of bacterial cell
It is 77%.
The layering MXene-Ti of preparation3C2With progress bacterial cell fluorescent staining, fluorescent staining figure after bacterium co-incubation 3h
As shown in Figure 10, wherein Fig. 7 is the fluorescent staining figure of bacterial cell, and Fig. 8 is the fluorescent staining figure of apoptotic bacteria cell.From Fig. 7-
It can be seen that after exposure 3h in 8 and Figure 11, normal bacteria bacterial cell proportion is much larger than apoptotic bacteria cell (arrow institute
It is normal bacterial cells to refer to), illustrate the obtained layering MXene-Ti after water is ultrasonically treated as layering agent3C2Only have
Weaker bactericidal effect.
Comparative example 2
(1) by 1g MXene-Ti3C2Powder is dispersed in 100ml dimethyl sulfoxide (DMSO)s (DMSO), in magnetic stirring apparatus
In stir 18h at 25 DEG C；
(2) after reaction, throw aside supernatant after acquired solution being centrifuged 15min under the rotating speed of 3500rpm, spend from
Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 2 times；
(3) obtained sediment is dispersed in 500ml deionized waters, is ultrasonically treated under the conditions of argon gas
(power is 100% and frequency is 45k Hz) 6h；
(4) solution after supersound process is uniformly poured into surface plate, the vacuum under room temperature in vacuum drying chamber
Drying for 24 hours, obtains layering MXene-Ti3C2Material
The layering MXene-Ti of preparation3C2The XRD spectra of material is not as shown in Figure 1, with MXene-Ti is layered3C2XRD
Spectrogram is compared, the layering MXene-Ti of preparation3C2Material does not generate apparent displacement；The layering MXene-Ti of preparation3C2Material
Interlamellar spacing and lattice constant are as shown in table 1, and are not layered MXene-Ti3C2Interlamellar spacing and lattice constant compare, it is only only light
Micro- increase shows that DMSO can play certain lamination, but inefficient.
The layering MXene-Ti of preparation3C2The anti-microbial property of material is as shown in Figure 5 and Figure 6, by the MXene-Ti of layering3C2
It is dispersed in the mother liquor for being configured to 2mg/ml in deionized water, Escherichia coli are exposed to the layering MXene- of various concentration
Ti3C2The middle culture different time takes the bacterium solution after culture to carry out being serially diluted tablet numeration, calculates the mistake of Bacillus coli cells
Motility rate, as a result as shown in Figure 5 and Figure 6, prepared layering MXene-Ti3C2Material has certain antibiotic property, and antibiotic property
Time-and concentration-dependent is presented, but antibiotic property is significantly lower than the layering MXene-Ti that isopropylamine or hydrazine hydrate are layered3C2Material
Material, slightly above the layering MXene-Ti of water stratification3C2Material, cell inactivation rate after exposure 5h can be only achieved 90%, and concentration reaches
It is only 84% to the activity suppression of bacterial cell when 200ug/mL.
The layering MXene-Ti of preparation3C2With progress bacterial cell fluorescent staining, fluorescent staining figure after bacterium co-incubation 3h
As shown in figure 12, wherein Fig. 7 is the fluorescent staining figure of bacterial cell, and Fig. 8 is the fluorescent staining figure of apoptotic bacteria cell.From Fig. 7-
It can be seen that after exposure 3h in 8 and Figure 12, normal bacteria bacterial cell proportion is much larger than apoptotic bacteria cell (arrow institute
It is normal bacterial cells to refer to), illustrate DMSO as obtained layering MXene-Ti after layering agent supersound process3C2Only have compared with
Weak bactericidal effect.
Comparative example 3
The MXene-Ti not being layered3C2。
Layering MXene-Ti prepared by 1 embodiment 1-6 of table and comparative example 1-33C2Or it is not layered MXene-Ti3C2Lattice
Constant and interlamellar spacing parameter
The present invention is inserted into MXene-Ti using hydrazine hydrate or isopropylamine3C2Interlayer, MXene- can be significantly increased
Ti3C2Interlamellar spacing and lattice constant, reduce lamellar spacing, after be allowed to remove layer by layer by way of supersound process, layering effect
Fruit is good；Layering MXene-Ti provided by the invention3C2For two-dimensional layer material, its antibiotic property is improved, antibiotic property is better than tradition
Two-dimension nano materials graphene has further widened two-dimensional layer MXene-Ti3C2The application field of material.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention,
Every technology and methods according to the present invention any simple modification, equivalent change and modification substantially made to the above embodiment,
In the range of the technology and methods scheme for still falling within the present invention.
Claims (8)
1. a kind of layering MXene-Ti improving antibiotic property3C2Preparation method, include the following steps：
(1) by Ti3AlC2- MAX phase ceramics powder and the mixing of HF solution, obtained mixed liquor are stirred to react under the conditions of oil bath, instead
Intermediate solution is obtained after answering；
(2) intermediate solution is subjected to washing centrifugation using deionized water, until pH=5~6 of supernatant；Continue to be carried out with ethyl alcohol
Washing centrifugation obtains sediment, is dried later, obtains MXene-Ti3C2Powder；
(3) MXene-Ti that will be obtained in step (2)3C2The solution of powder and hydrazine hydrate or isopropylamine is sufficiently mixed stirring, stirs
Intermediate solution is obtained after reaction；
(4) intermediate solution obtained in step (3) is ultrasonically treated, the solution filter membrane mistake being ultrasonically treated after terminating
Filter is improved the layering MXene-Ti of antibiotic property after dry3C2。
2. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
The mass concentration of HF solution is 40~49% in step (1).
3. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
Ti in step (1)3AlC2The rate of charge of-MAX phase ceramics powder and HF solution is 1g:16~24ml.
4. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
MXene-Ti in step (3)3C2The rate of charge of powder and hydrazine hydrate is 1g:80~120ml.
5. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
MXene-Ti in step (3)3C2The rate of charge of powder and isopropyl amine aqueous solution is 1g：80~120ml, the isopropyl amine aqueous solution
Volumetric concentration is 15~25%.
6. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
The step of (3) in MXene-Ti3C2Powder is mixed with hydrazine hydrate, the layering MXene-Ti that step (4) obtains3C2Lattice constant
ForInterlamellar spacing isLamellar spacing is 21-27nm.
7. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
The step of (3) in MXene-Ti3C2Powder is mixed with isopropylamine, the layering MXene-Ti that step (4) obtains3C2Lattice constant
ForInterlamellar spacing isLamellar spacing is 10-17nm.
8. the layering MXene-Ti according to claim 1 for improving antibiotic property3C2Preparation method, which is characterized in that it is described
The step of (4) in frequency for being ultrasonically treated be 40~50kHz, the power of supersound process is 80~100%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810420678.3A CN108584959B (en) | 2018-05-04 | 2018-05-04 | Preparation method of layered two-dimensional transition metal carbide or carbonitride-titanium dicarbonide for improving antibacterial property |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810420678.3A CN108584959B (en) | 2018-05-04 | 2018-05-04 | Preparation method of layered two-dimensional transition metal carbide or carbonitride-titanium dicarbonide for improving antibacterial property |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108584959A true CN108584959A (en) | 2018-09-28 |
| CN108584959B CN108584959B (en) | 2020-04-28 |
Family
ID=63620851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810420678.3A Active CN108584959B (en) | 2018-05-04 | 2018-05-04 | Preparation method of layered two-dimensional transition metal carbide or carbonitride-titanium dicarbonide for improving antibacterial property |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108584959B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603556A (en) * | 2018-12-12 | 2019-04-12 | 浙江工业大学 | Preparation method of mixed matrix membrane based on MXene material |
| CN111285359A (en) * | 2020-01-14 | 2020-06-16 | 武汉理工大学 | Preparation method of single-layer/few-layer MXene two-dimensional material |
| CN111808841A (en) * | 2020-07-30 | 2020-10-23 | 香港大学深圳医院 | Method for eliminating antibiotic resistance of drug-resistant escherichia coli |
| CN113083213A (en) * | 2021-04-07 | 2021-07-09 | 西南科技大学 | Single-layer MXene colloid and preparation method and application thereof |
| CN115058169A (en) * | 2022-02-07 | 2022-09-16 | 西北工业大学 | MXene-based anticorrosive and antifouling composite coating and preparation method and application thereof |
| CN115177791A (en) * | 2021-04-02 | 2022-10-14 | 苏州北科纳米科技有限公司 | Preparation and application of MXenes biological coating with good biocompatibility |
| CN115569147A (en) * | 2022-09-29 | 2023-01-06 | 浙江瑞邦药业股份有限公司 | Preparation method and application of platinum monatomic supported MXene nanosheet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817083A (en) * | 2015-05-25 | 2015-08-05 | 哈尔滨工业大学 | Rapid-heating-assisted ultrasonic stripping method for two-dimensional nanometer Ti3C2 lamella |
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN107324335A (en) * | 2017-08-17 | 2017-11-07 | 浙江大学 | A kind of utilization ultrasonic wave added prepares the Mxene Ti of layering3C2Method |
-
2018
- 2018-05-04 CN CN201810420678.3A patent/CN108584959B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817083A (en) * | 2015-05-25 | 2015-08-05 | 哈尔滨工业大学 | Rapid-heating-assisted ultrasonic stripping method for two-dimensional nanometer Ti3C2 lamella |
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN107324335A (en) * | 2017-08-17 | 2017-11-07 | 浙江大学 | A kind of utilization ultrasonic wave added prepares the Mxene Ti of layering3C2Method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603556A (en) * | 2018-12-12 | 2019-04-12 | 浙江工业大学 | Preparation method of mixed matrix membrane based on MXene material |
| CN111285359A (en) * | 2020-01-14 | 2020-06-16 | 武汉理工大学 | Preparation method of single-layer/few-layer MXene two-dimensional material |
| CN111808841A (en) * | 2020-07-30 | 2020-10-23 | 香港大学深圳医院 | Method for eliminating antibiotic resistance of drug-resistant escherichia coli |
| CN115177791A (en) * | 2021-04-02 | 2022-10-14 | 苏州北科纳米科技有限公司 | Preparation and application of MXenes biological coating with good biocompatibility |
| CN113083213A (en) * | 2021-04-07 | 2021-07-09 | 西南科技大学 | Single-layer MXene colloid and preparation method and application thereof |
| CN115058169A (en) * | 2022-02-07 | 2022-09-16 | 西北工业大学 | MXene-based anticorrosive and antifouling composite coating and preparation method and application thereof |
| CN115569147A (en) * | 2022-09-29 | 2023-01-06 | 浙江瑞邦药业股份有限公司 | Preparation method and application of platinum monatomic supported MXene nanosheet |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108584959B (en) | 2020-04-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108584959A (en) | A kind of preparation method for being layered two-dimentional transition metal carbide or the carbonization Tritanium/Trititanium of carbonitride-two improving antibiotic property | |
| Jia et al. | Versatile graphene-based photothermal nanocomposites for effectively capturing and killing bacteria, and for destroying bacterial biofilms | |
| CN103881124B (en) | Polyamide layer of a kind of load stannic oxide/graphene nano thin slice and its preparation method and application | |
| CN104497344B (en) | A kind of method being modified to polyether-ether-ketone surface | |
| CN104629067B (en) | A kind of preparation method for regenerating the plain composite membrane of polyvinyl alcohol of antibiotic fiber | |
| CN104839210A (en) | Preparation method and application for magnetic-nanosilver-graphene nano composite material l | |
| CN107540882A (en) | A kind of preparation method and application of multi function shell glycan composite sponge | |
| CN109809481B (en) | Method for preparing titanium dioxide polyhedron with hollow structure by using titanium carbide ultrathin nanosheets | |
| TWI398276B (en) | Method for producing bacterial cellulose with controlled pore size and its use in wound dressing | |
| CN104927097B (en) | A kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites | |
| CN113244793B (en) | Preparation and application of durable high-flux emulsion separation membrane material | |
| CN114163817A (en) | Slow-release antibacterial film and preparation method thereof | |
| CN112516975A (en) | Anti-biological fouling type hydrogel film material for extracting uranium from seawater and preparation method thereof | |
| CN109938038B (en) | Graphene oxide antibacterial liquid for biology and preparation method thereof | |
| WO2022165877A1 (en) | Malic acid-chitosan nanopore hydrogel microsphere, and preparation method therefor and application thereof | |
| Yang et al. | Polyacrylamide grafted cellulose as an eco-friendly flocculant: efficient removal of organic dye from aqueous solution | |
| CN106582492A (en) | ZrO2 for heavy metal wastewater treatment and preparation method and application thereof | |
| Zhang et al. | Fabrication of macroporous titanium dioxide film using PMMA microspheres as template | |
| CN107188207B (en) | A kind of preparation method for the magnesium oxide material being assembled into micron bar structure by nanometer sheet | |
| CN108585100A (en) | A method of adsorbing water Malachite Green using metal-organic framework materials MIL-100 (Fe) | |
| CN106178008B (en) | A kind of ultrasound-piezoelectricity Synergistic biocidal technology | |
| CN1261356C (en) | Biomimetic mintralization in situ preparation method of functional nanometer calcium carbonate | |
| CN113976080B (en) | Preparation method of two-dimensional material and method for adsorbing phosphorus in water by using two-dimensional material | |
| CN110354313A (en) | A kind of magnetic enhancement phase modified composite material and preparation method thereof | |
| CN109972385A (en) | A kind of surface treatment method of bamboo and woods fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |