CN105253882B - Ultra-dispersed antimicrobial nano diamond and preparation method thereof - Google Patents
Ultra-dispersed antimicrobial nano diamond and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of ultra-dispersed antimicrobial nano diamond and preparation method thereof.Step includes：Nano diamond original powder is subjected to mechanical lapping, obtains the Nano diamond aggregate of homogeneous grain diameter；Nano diamond after grinding is dispersed in ethanol solution；The reaction of the bromopropyl trimethoxy silane of silane coupler 3 is added into Nano diamond ethanol solution obtained by step b, washing separation drying, obtains silanization Nano diamond after reaction terminates；Silanization Nano diamond is scattered in solvent, and adds poly- tetravinyl pyridine and brominated alkanes and is reacted, by reaction product using ether precipitation, washing, dry the quaternized Nano diamond of end-product after centrifugation.The Nano diamond of the stable dispersion in water can be obtained by this kind of chemical modification method, increase its mechanical property in composite as additive application, applied to biologic medical field as pharmaceutical carrier, it simultaneously can be used for dental restorative area and make anti-biotic material.
Description
Technical field
The invention belongs to Diamond machining techniques field, particularly a kind of ultra-dispersed antimicrobial nano diamond and its system
Preparation Method.
Background technology
Because Nano diamond has excellent mechanics, optics, electricity, thermal property, distinctive chemical stability, surface
Abundant modifies functional group, and good biocompatibility, and in precise finiss, material, biologic medical field has potential
Application value.Diamond particles granularity prepared by detonation synthesis is typically equal in below 10nm, grain shape rule, granularity
It is even, but because nano-particle has large specific surface area and higher specific surface energy, and Nano diamond surface is contained largely
Functional group, make it easily assemble to form aggregate.Current to bombard that method synthetic technology is more ripe, obtained Nano diamond has
Unique physical and chemical properties, but if de-agglomerated problem and in the solution stability can not solve very well, nanometer Buddha's warrior attendant
The superior performance of stone cannot just play, and limit its popularization and application.
The method of existing Nano diamond de-agglomerated has Physical and chemical method.Li etc. (non-patent literature) is first to nanometer Buddha's warrior attendant
Stone carries out the pre-heat treatment, after ball milling and surfactant combined into carry out decentralized processing, the Nano diamond finally given
Trimestral stable dispersion can be kept in butanone or acetone and other organic solvent.CN102391789A Chinese patent literatures handle is received
Rice diamond is placed in the ball grinder of high energy ball mill, addition grinding aid polyethylene glycol, dispersant op-10 and deionized water,
Wet ball grinding is carried out by medium of water, then again through over cleaning and acid treatment, the particle diameter that finally classification obtains Nano diamond is
10~100nm.Zhu etc. (non-patent literature) first adds the agitation of anions and canons surfactant and then uses ceramics and stainless steel ball
Grinding and the simultaneously hyper-dispersant such as addition, make surface group become hydrophobic group by hydrophilic group, finally prepare the lightweight that granularity is
Oil dispersion liquid.CN1439451A Chinese patent literatures by ultrasound and ball milling means, and add simultaneously appropriate ion and
Nonionic surfactant, diamond stable dispersion in water can be made, particle diameter is substantially in below 100nm.
Find that either Physical or chemical method improve dispersion stabilization to diamond de-agglomerated from the research of forefathers
The step of and process more trouble it is complicated, it is necessary to add dispersant, surfactant in the solution so as to improve dispersion stabilization,
Nano diamond dispersing characteristic is not changed inherently by the modification of diamond surface chemical group.At present, do not have also
The dispersiveness and anti-microbial property of Nano diamond are included research category by correlative study simultaneously, and the field belongs to a blank.
The content of the invention
It is an object of the invention to provide a kind of diamond hydration size controlling can be made ultra-dispersed in smaller range
Antimicrobial nano diamond and preparation method thereof, assign Nano diamond anti-microbial property, and for Nano diamond in difference
The application in field provides broad space.
The technical solution for realizing the object of the invention is：A kind of preparation side of ultra-dispersed antimicrobial nano diamond
Method, comprise the following steps：
A. Nano diamond original powder is subjected to mechanical lapping, obtains the Nano diamond aggregate of homogeneous grain diameter；
B. the Nano diamond after grinding is dispersed in ethanol solution；
C. it is anti-that silane coupler 3- bromopropyl trimethoxy silanes are added into Nano diamond ethanol solution obtained by step b
Should, washing separation drying, obtains silanization Nano diamond after reaction terminates；
D. silanization Nano diamond is scattered in solvent, and adds poly- tetravinyl pyridine and brominated alkanes and carry out instead
Should, by reaction product using ether precipitation, washing, dry the quaternized Nano diamond of end-product after centrifugation.
Preferably, Nano diamond original powder described in step a is obtained by Detonation Process, and hydration particle diameter is 350.3nm.
Preferably, the volume ratio of alcohol to water of ethanol solution is (8~9.5) in step b:1.
Preferably, the Nano diamond described in step c in Nano diamond ethanol solution and 3- bromopropyl trimethoxies
The mass ratio of silane is 100:(10~1), 40 DEG C~60 DEG C of reaction temperature, reaction time 16h~24h.
Preferably, solvent described in step d is nitromethane, dimethyl sulfoxide (DMSO) or dimethylformamide；Silanization nanometer
The mass ratio of diamond and poly- tetravinyl pyridine, brominated alkanes is 1:5:(0~4).
Preferably, brominated alkanes described in step d are bromoethane, N-Propyl Bromide, NBB, bromo pentane silane or bromohexane.
Preferably, silanization Nano diamond is scattered in solvent described in step d, and add poly- tetravinyl pyridine and
Brominated alkanes are reacted, and reaction temperature is 50 DEG C~70 DEG C, reaction time 16h~24h.
The ultra-dispersed antimicrobial nano diamond that a kind of as above either method prepares gained is quaternized Nano diamond.
Compared with prior art, its remarkable advantage is the present invention：(1) obtain Nano diamond hydration particle diameter it is smaller
Within 200nm, and in aqueous can long-time stable disperse, coagulation does not occur；(2) Nano diamond yield is higher, reaches
To more than 85%；(3) Nano diamond has antibacterial action, has further widened the application field of Nano diamond；(4) technology
Technique is simple, and raw material is easy to get, and does not produce destruction to environment, and liquid waste processing is simple, is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of Nano diamond original powder of the present invention.
Fig. 2 is that Nano diamond original powder of the present invention is hydrated grain size distribution.
Fig. 3 is the INFRARED SPECTRUM of Nano diamond original powder, silanization and quaternized Nano diamond in the embodiment of the present invention 1
Figure.
Fig. 4 is the transmission electron microscope picture of quaternized Nano diamond in the embodiment of the present invention 1.
Fig. 5 is the grain size distribution of quaternized Nano diamond in the embodiment of the present invention 1.
Embodiment
The preparation method of the ultra-dispersed antimicrobial nano diamond of the present invention, comprises the following steps：
A. Nano diamond original powder is subjected to mechanical lapping, obtains the Nano diamond aggregate of homogeneous grain diameter；
B. the Nano diamond after grinding is dispersed in ethanol solution；
C. it is anti-that silane coupler 3- bromopropyl trimethoxy silanes are added into Nano diamond ethanol solution obtained by step b
Should, washing separation drying, obtains silanization Nano diamond after reaction terminates；
D. silanization Nano diamond is scattered in solvent, and adds poly- tetravinyl pyridine and brominated alkanes and carry out instead
Should, by reaction product using ether precipitation, washing, dry the quaternized Nano diamond of end-product after centrifugation.
Preferably, Nano diamond original powder described in step a is obtained by Detonation Process, and hydration particle diameter is 350.3nm.Step a
The larger Nano diamond aggregate of middle mechanical lapping makes granularity compared with small agglomerates, is advantageous to disperse in the solution with after
The abundant haptoreaction of continuous reactant.
Preferably, the volume ratio of alcohol to water of ethanol solution is (8~9.5) in step b:1, under conditions of a small amount of water, silane
Coupling agent can hydrolyze.
Preferably, the Nano diamond described in step c in Nano diamond ethanol solution and 3- bromopropyl trimethoxies
The mass ratio of silane is 100:(10~1), 40 DEG C~60 DEG C of reaction temperature, reaction time 16h~24h.
Preferably, solvent described in step d is nitromethane, dimethyl sulfoxide (DMSO) or dimethylformamide；Silanization nanometer
The mass ratio of diamond and poly- tetravinyl pyridine, brominated alkanes is 1:5:(0~4).The increase of brominated alkanes quality, quaternized journey
Degree is improved, and Nano diamond dispersiveness and anti-microbial property in water get a promotion.
Preferably, brominated alkanes described in step d are bromoethane, N-Propyl Bromide, NBB, bromo pentane silane or bromohexane.With
The increase of bromo alkyl chain length, the hydrophobicity enhancing (hydrophily of quaternized Nano diamond：Bromoethane>N-Propyl Bromide>NBB>
Bromo pentane silane>Bromohexane), but anti-microbial property is improved (anti-microbial property：Bromohexane>Bromo pentane silane>NBB>N-Propyl Bromide>Bromine second
Alkane).
Preferably, silanization Nano diamond is scattered in solvent described in step d, and add poly- tetravinyl pyridine and
Brominated alkanes are reacted, and reaction temperature is 50 DEG C~70 DEG C, reaction time 16h~24h.
The ultra-dispersed antimicrobial nano diamond that a kind of as above either method prepares gained is quaternized Nano diamond,
It can be used in the fields such as composite, biologic medical, dental prosthetic material.
Embodiment 1
Step a：With mortar by Nano diamond mechanical lapping, wherein larger aggregate is set to be dispersed into granularity more uniform
Small agglomerates, it is characterized by transmission electron microscope and dynamic light scattering particle size instrument, such as Fig. 1 and Fig. 2, hydration particle diameter 350.3nm；
Step b：The Nano diamond after 2g grindings is weighed to be dispersed in the ethanol solution of 100mL mass fractions 80%；
Step c：The 3- bromopropyls trimethoxy silane of Nano diamond quality 5% is added into above-mentioned system instead in 40 DEG C
At a temperature of react 16h after, with ethanol wash filter drying, obtain silanization Nano diamond, it characterized by infrared, such as figure
3；
Step d：Weigh 60mg silanization Nano diamonds to be scattered in solvent nitromethane, add the poly- tetravinyls of 0.3g
Pyridine and 0.12g bromohexanes (silanization Nano diamond：Poly- tetravinyl pyridine：Bromohexane=1:5:2) at a temperature of 50 DEG C
After reacting 24h, in ether washing of precipitate centrifuge dry the quaternized Nano diamond of end-product, such as Fig. 4 and Fig. 5, water
Close particle diameter 167.5nm.
Obtain quaternized Nano diamond can long-time stable in water disperse, by observe Nano diamond original powder,
Silanization Nano diamond and the quaternized Nano diamond of final modified product disperse photo in water after 7 days, it is known that quaternized
Nano diamond long-time stable can disperse in water.
In addition, it is 10 to bacterium colony concentration to test quaternized Nano diamond7CFU/mL Escherichia coli antibacterial activity, is obtained
It is respectively 15.6 μ g/mL and 31.2 μ g/mL to minimal inhibitory concentration (MIC) and minimum bactericidal concentration (MBC), there is good resist
Bacterium performance.
Embodiment 2~12 gives the ethanol solution of different quality containing, different 3- bromines according to the experimental method of embodiment 1
Propyl trimethoxy silicane mass fraction, differential responses temperature and reaction time, and different brominated alkanes account for reaction system
In the case of mass ratio, the different quaternization degree Nano diamonds of acquisition.
Embodiment 2
Step b：The ethanol solution of mass fraction 80%；
Step c：The 3- bromopropyls of Nano diamond quality 5% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 16h, 40 DEG C of reaction temperature；
Step d：Solvent is nitromethane, silanization Nano diamond：Poly- tetravinyl pyridine：Bromohexane=1:5:0, instead
Temperature 50 C is answered, reacts 24h.
Embodiment 3
Step b：The ethanol solution of mass fraction 80%；
Step c：The 3- bromopropyls of Nano diamond quality 5% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 16h, 40 DEG C of reaction temperature；
Step d：Solvent is nitromethane, silanization Nano diamond：Poly- tetravinyl pyridine：Bromohexane=1:5:1, instead
Temperature 50 C is answered, reacts 24h.
Embodiment 4
Step b：The ethanol solution of mass fraction 85%；
Step c：The 3- bromopropyls of Nano diamond quality 5% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 16h, 40 DEG C of reaction temperature；
Step d：Solvent is nitromethane, silanization Nano diamond：Poly- tetravinyl pyridine：Bromohexane=1:5:4, instead
Temperature 50 C is answered, reacts 24h.
Embodiment 5
Step b：The ethanol solution of mass fraction 90%；
Step c：The 3- bromopropyls of Nano diamond quality 5% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 20h, 50 DEG C of reaction temperature；
Step d：Solvent is dimethyl sulfoxide (DMSO), silanization Nano diamond：Poly- tetravinyl pyridine：Bromoethane=1:5:2,
60 DEG C of reaction temperature, react 20h.
Embodiment 6
Step b：Measure the ethanol solution matter of fraction 90%；
Step c：The 3- bromopropyls of Nano diamond quality 10% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 20h, 50 DEG C of reaction temperature；
Step d：Solvent is dimethyl sulfoxide (DMSO), silanization Nano diamond：Poly- tetravinyl pyridine：Bromoethane=1:5:4,
60 DEG C of reaction temperature, react 20h.
Embodiment 7
Step b：The ethanol solution of mass fraction 90%；
Step c：The 3- bromopropyls of Nano diamond quality 10% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 20h, 50 DEG C of reaction temperature；
Step d：Solvent is dimethyl sulfoxide (DMSO), silanization Nano diamond：Poly- tetravinyl pyridine：N-Propyl Bromide=1:5:2,
60 DEG C of reaction temperature, react 20h.
Embodiment 8
Step b：The ethanol solution of mass fraction 90%；
Step c：The 3- bromopropyls of Nano diamond quality 10% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 20h, 50 DEG C of reaction temperature；
Step d：Solvent is dimethyl sulfoxide (DMSO), silanization Nano diamond：Poly- tetravinyl pyridine：N-Propyl Bromide=1:5:4,
60 DEG C of reaction temperature, react 20h.
Embodiment 9
Step b：The ethanol solution of mass fraction 95%；
Step c：The 3- bromopropyls of Nano diamond quality 1% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 24h, 60 DEG C of reaction temperature, reaction time 24h；
Step d：Solvent is dimethylformamide, silanization Nano diamond：Poly- tetravinyl pyridine：NBB=1:5:
2,70 DEG C of reaction temperature, react 16h.
Embodiment 10
Step b：The ethanol solution of mass fraction 95%；
Step c：The 3- bromopropyls of Nano diamond quality 1% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 24h, 60 DEG C of reaction temperature, reaction time 24h；
Step d：Solvent is dimethylformamide, silanization Nano diamond：Poly- tetravinyl pyridine：NBB=1:5:
4,70 DEG C of reaction temperature, react 16h.
Embodiment 11
Step b：The ethanol solution of mass fraction 95%；
Step c：The 3- bromopropyls of Nano diamond quality 3% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 24h, 60 DEG C of reaction temperature；
Step d：Solvent is dimethylformamide, silanization Nano diamond：Poly- tetravinyl pyridine：Bromo pentane silane=1:5:
2,70 DEG C of reaction temperature, react 16h.
Embodiment 12
Step b：The ethanol solution of mass fraction 95%；
Step c：The 3- bromopropyls of Nano diamond quality 3% are added into Nano diamond ethanol solution obtained by step b
Trimethoxy silane reacts 24h, 60 DEG C of reaction temperature；
Step d：Solvent is dimethylformamide, silanization Nano diamond：Poly- tetravinyl pyridine：Bromo pentane silane=1:5:
4,70 DEG C of reaction temperature, react 16h.
Embodiment 13
After tested, table 1 list quaternized diamond minimal inhibitory concentration, minimum bactericidal concentration that embodiment 1~12 provides,
It is hydrated stable dispersion number of days in particle diameter and water.
Table 1
Note："-" is represented substantially without anti-microbial property
Because Nano diamond has the hardness of superelevation, stability and biocompatibility are increasingly by researcher
Favor, particularly in antibacterial field.Nano diamond does not have anti-microbial property in itself, but quaternary ammonium salt is as a kind of high-efficiency broad spectrum
Antiseptic is generally grafted on other materials and plays antibacterial action.Therefore, quaternary ammonium salt modification is arrived Nano diamond by the present invention
Surface, two kinds of material peculiar properties can be played complementation, using the enhancing for being related to Compound Material Engineering intensity, biological medicine carries
The fields such as body, dental prosthetic material.
Claims (8)
1. a kind of preparation method of ultra-dispersed antimicrobial nano diamond, it is characterised in that comprise the following steps：
A. Nano diamond original powder is subjected to mechanical lapping, obtains the Nano diamond aggregate of homogeneous grain diameter；
B. the Nano diamond after grinding is dispersed in ethanol solution；
C. the reaction of silane coupler 3- bromopropyls trimethoxy silane is added into Nano diamond ethanol solution obtained by step b,
Washing separation drying, obtains silanization Nano diamond after reaction terminates；
D. silanization Nano diamond is scattered in solvent, and adds poly- tetravinyl pyridine and brominated alkanes and reacted,
By reaction product using ether precipitation, washing, dry the quaternized Nano diamond of end-product after centrifugation.
2. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 1, it is characterised in that step a
Described in Nano diamond original powder obtained by Detonation Process, hydration particle diameter is 350.3nm.
3. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 1, it is characterised in that step b
The volume ratio of alcohol to water of middle ethanol solution is (8~9.5):1.
4. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 1, it is characterised in that step c
Described in the mass ratio of Nano diamond in Nano diamond ethanol solution and 3- bromopropyl trimethoxy silanes be 100:(10
~1), 40 DEG C~60 DEG C of reaction temperature, reaction time 16h~24h.
5. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 1, it is characterised in that step d
Described in solvent be nitromethane, dimethyl sulfoxide (DMSO) or dimethylformamide；Silanization Nano diamond and poly- tetravinyl pyrrole
Pyridine, the mass ratio of brominated alkanes are 1:5:(1~4).
6. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 1 or 5, it is characterised in that step
Brominated alkanes are bromoethane, N-Propyl Bromide, NBB, bromo pentane silane or bromohexane described in rapid d.
7. the preparation method of ultra-dispersed antimicrobial nano diamond according to claim 6, it is characterised in that step d
It is described that silanization Nano diamond is scattered in solvent, and add poly- tetravinyl pyridine and brominated alkanes and reacted, instead
It is 50 DEG C~70 DEG C to answer temperature, reaction time 16h~24h.
8. a kind of ultra-dispersed antimicrobial nano diamond that gained is prepared such as claim 1~7 either method is quaternized receives
Rice diamond.
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| CN107440912A (en) * | 2017-08-03 | 2017-12-08 | 无锡南理工科技发展有限公司 | The preparation method of dental prosthetic material |
| CN107616923A (en) * | 2017-09-06 | 2018-01-23 | 无锡南理工科技发展有限公司 | The preparation method of titanium-based dental prosthetic material |
| CN107711828A (en) * | 2017-09-15 | 2018-02-23 | 南京理工大学 | Silver/cation copolymer modified Nano diamond compound particle and preparation method thereof |
| WO2020026790A1 (en) * | 2018-07-30 | 2020-02-06 | 株式会社ダイセル | Surface-modified nanodiamond and dispersion and composite material containing surface-modified nanodiamond |
| CN109403021B (en) * | 2018-10-31 | 2021-04-16 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Nano carbon crystal pure cotton surface antibacterial fiber and preparation method thereof |
| CN112980231A (en) * | 2021-03-05 | 2021-06-18 | 物生生物科技(北京)有限公司 | Surface modification method of nano hard particles with antibacterial performance |
| CN114988403A (en) * | 2022-06-30 | 2022-09-02 | 华中师范大学 | Liquid phase preparation method and application of aminated nano-diamond redispersed in solvent |
| CN116254146A (en) * | 2023-02-01 | 2023-06-13 | 长治市龙晨科技有限公司 | Water-based diamond cutting fluid and preparation method thereof |
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| CN1186401C (en) * | 2002-05-17 | 2005-01-26 | 中山大学 | Nano diamond particle surface treatment method |
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