CN105707122B - A kind of nano composite antibiotic material and its preparation method and application - Google Patents
A kind of nano composite antibiotic material and its preparation method and application Download PDFInfo
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- CN105707122B CN105707122B CN201610049313.5A CN201610049313A CN105707122B CN 105707122 B CN105707122 B CN 105707122B CN 201610049313 A CN201610049313 A CN 201610049313A CN 105707122 B CN105707122 B CN 105707122B
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
The invention discloses a kind of nano composite antibiotic material and its preparation method and application, vanadic anhydride and pucherite that the anti-biotic material is 0.30~1.50 by molar ratio form；The preparation method, includes the following steps：1) hydrochloric acid is added dropwise to NH4VO3It in solution, is then added dropwise in hydrazine hydrate solution again, after being stirred at room temperature, suction filtration obtains reaction product；2) Bi (NO and then by the reaction product are added to3)3·5H2Ultrasonic mixing in O solution, then it is alkalinity that ammonium hydroxide, which is added dropwise, to be adjusted to the pH value of reaction system, obtains reaction mixture, then the reaction mixture is stirred to react, obtains filter cake；3) again will after the filtration cakes torrefaction, roast to get；The application is application of the anti-biotic material in being used to prepare antibacterials.The nanocomposite of gained of the invention has antibacterial functions.
Description
Technical field
The present invention relates to a kind of anti-biotic materials and its preparation method and application, and in particular to a kind of nano composite antibiotic material
And its preparation method and application.
Background technology
With the general advance of human society, people become more concerned with environmental problem, reduce and effectively prevent living environment
Middle microorganism is increasingly becoming thus germ infection that interference and harm, the mitigation of human lives cause the common recognition of society.
In the numerous measures for controlling environmental microorganism, inorganic antibacterial is because having many advantages, such as special efficacy, safety and health as numerous control
The means of microorganism.Especially in recent years with nano-TiO2It is found to be a kind of good fungicide for the photochemical catalyst of representative,
It can not only effectively kill bacterium, and the compound released by bacterium that can degrade simultaneously, have extensively in many antibacterial fields
Wealthy application prospect.But nano-photo catalytic sterilization material does not often have antibiotic property under conditions of no light or low-light
Can, the application this greatly limits this kind of catalysis material in antibacterial field.
Nano inorganic composite material has obtained greatly developing in recent years.Compound material can be assigned by nano level more
The comprehensive performance added solves single structure inorganic functional material and is applying upper limitation, improves material property and application range.
For example, light induced electron-sky can be improved by the heterojunction structure of two kinds of inorganic semiconductor nanometer materials being effectively compounded to form
Cave separative efficiency greatly improves material light catalysis germicidal efficiency.If using nanometer composite technology to existing photo-catalyst material
Material carries out composite modified, sterilization of the raising composite material under non-illuminated conditions while reserved materials photo-catalyst performance
Performance will greatly expand application of such material in antibacterial field.
Invention content
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of nano composite antibiotic material and its preparation sides
Method and application, so as to effectively solve the inorganic sterilization material of traditional photocatalysis under non-illuminated conditions without bactericidal property or bactericidal properties
The weak technical barrier of energy.
In order to achieve the above objectives, technical scheme is as follows：
On the one hand, the present invention provides a kind of nano composite antibiotic material, by five oxidations two that molar ratio is 0.30~1.50
Vanadium and pucherite composition.
Based on the above technical solution, the present invention can also make following improvement：
As a preferred option, the vanadic anhydride and pucherite that the nano composite antibiotic material is 1.44 by molar ratio
Composition.
On the other hand, the present invention also provides a kind of preparation method of above-mentioned nano composite antibiotic material, include the following steps：
1) hydrochloric acid is added dropwise to NH4VO3It in solution, is then added dropwise in hydrazine hydrate solution, after being stirred at room temperature, filters again
Obtain reaction product；
2) Bi (NO and then by the reaction product are added to3)3·5H2Ultrasonic mixing in O solution, then ammonium hydroxide is added dropwise and is adjusted to
The pH value of reaction system is alkalinity, obtains reaction mixture, then the reaction mixture is stirred to react, obtains filter cake；
3) again will after the filtration cakes torrefaction, roast to get.
Based on the above technical solution, the present invention can also make following improvement：
As a preferred option, in step 1), by 0.5~2.0mL, 0.5~2.0mol/L hydrochloric acid is added dropwise to 0.03~
The NH of 0.06mol/L4VO3In solution, it is then added dropwise 4~12mL again, in the hydrazine hydrate solution of 80 volume %, is stirred at room temperature
20~40min, suction filtration obtain reaction product.
As a preferred option, by 1mL, 1mol/L hydrochloric acid is added dropwise to the NH of 0.05mol/L4VO3In solution, then again by
It is added dropwise to 6mL, in 80% hydrazine hydrate solution, 30min is stirred at room temperature, suction filtration obtains reaction product.
As a preferred option, in step 2), the reaction product is added to 100mL, 0.001~0.02mol/L
Bi (NO3)3·5H220~40min of ultrasonic mixing in the reaction product is added in O solution, and ammonium hydroxide is added dropwise and is adjusted to reaction system
PH value 9~10 obtains reaction mixture, then the reaction mixture is stirred 0.5~2h, obtains filter cake.
As a preferred option, by 100mL, the Bi (NO of 0.005mol/L3)3·5H2The reaction product is added in O solution
Middle ultrasound mixing 30min, is added dropwise the pH value 10 that ammonium hydroxide is adjusted to reaction system, obtains reaction mixture, then the reaction is mixed
Object is stirred to react 1 hour, obtains filter cake.
As a preferred option, in step 3), the filter cake in 40~60 DEG C after dry 24 hours, 2~10 DEG C/
Under the heating rate of min, it is warming up to 300~500 DEG C of 1~5h of roasting heat preservation.
As a preferred option, the filter cake is after 60 DEG C are 24 hours dry, under the heating rate of 5 DEG C/min, heating
To 400 DEG C of roasting heat preservation 2h.
Further aspect, the present invention also provides a kind of above-mentioned nano composite antibiotic material answering in being used to prepare antibacterials
With.
Even if the nano composite antibiotic material of the present invention still has good bactericidal property under non-illuminated conditions, having
Under illumination condition, sterilization rate faster, can effectively solve the inorganic sterilization material of traditional photocatalysis under non-illuminated conditions without sterilization
Performance or the weak technical barrier of bactericidal property, have broad prospect of application in antimicrobial technology field；And in specific reaction condition
Under, the anti-microbial property such as anti-biotic material obtained under reaction ratio is more excellent.
Description of the drawings
Fig. 1 is the XRD spectra for the nano combined sterilization material of vanadic anhydride/pucherite that the embodiment of the present invention 1 provides
(wherein 2 θ of abscissa-angle, unit are ° (degree)；Ordinate-intensity (Intensity), unit are a.u. (absolute unit)).
Fig. 2 is the XRD spectra for the nano combined sterilization material of vanadic anhydride/pucherite that the embodiment of the present invention 2 provides
(wherein 2 θ of abscissa-angle, unit are ° (degree)；Ordinate-intensity (Intensity), unit are a.u. (absolute unit)).
Fig. 3 is the XRD spectra for the nano combined sterilization material of vanadic anhydride/pucherite that the embodiment of the present invention 3 provides
(wherein 2 θ of abscissa-angle, unit are ° (degree)；Ordinate-intensity (Intensity), unit are a.u. (absolute unit)).
Fig. 4 is the XRD spectra for the nano combined sterilization material of vanadic anhydride/pucherite that the comparative example 1 of the present invention provides
(wherein 2 θ of abscissa-angle, unit are ° (degree)；Ordinate-intensity (Intensity), unit are a.u. (absolute unit)).
Fig. 5 is the XRD spectra for the nano combined sterilization material of vanadic anhydride/pucherite that the comparative example 2 of the present invention provides
(wherein 2 θ of abscissa-angle, unit are ° (degree)；Ordinate-intensity (Intensity), unit are a.u. (absolute unit)).
Fig. 6 be the nano combined sterilization material of vanadic anhydride/pucherite that provides of the embodiment of the present invention 2 have illumination and
To the killing rate of pseudomonas aeruginosa, (wherein abscissa-time Time, unit are min (minute) under non-illuminated conditions；It is vertical to sit
Mark-sterilizing rate (Antibacterial rate), unit are % (percentage)).
Specific implementation mode
Below in a manner of specific embodiment, the preferred embodiment of the present invention is further illustrated.
Unless specifically stated otherwise, reagent used in following embodiment is that analysis level is pure and obtained commercially available from regular channel
.
Embodiment 1
By NH4VO3Be configured to the aqueous solution of a concentration of 0.05mol/L, be added dropwise 1mL, in 1mol/L hydrochloric acid to system, after by
It is added dropwise to 6mL, 80 volume % hydrazine hydrates, suction filtration obtains product after 30min is stirred at room temperature.Then weigh suitable Bi (NO3)3·
5H2O, which is dissolved in 1mol/L nitric acid, is configured to 100ml, the aqueous solution of 0.005mol/L, is added and filters product ultrasound 30min, is added dropwise
Ammonium hydroxide is adjusted to pH value of reaction system 10, and magnetic agitation 1 hour is then washed with deionized water, ethyl alcohol successively, filtering, by filter cake
It is V to keep the temperature 2h in the heating rate of 5 DEG C/min to 400 DEG C of roastings up to chemical composition after being dried 24 hours at 60 DEG C2O5/BiVO4
Vanadic anhydride/pucherite nano composite antibiotic material.
The characterization of the nano combined sterilization material of vanadic anhydride/pucherite：
X-ray diffraction analysis is the result shows that contain only V in composite material2O5And BiVO4Two-phase (Fig. 1), passes through energy disperse spectroscopy
(EDS) it analyzes, the results showed that V in nano composite antibiotic material2O5/BiVO4Molar ratio be 1.44.
Embodiment 2
By NH4VO3It is configured to the aqueous solution of a concentration of 0.03mol/L, is added dropwise 0.5mL, in 2mol/L hydrochloric acid to system, after
4mL is added dropwise, 80 volume % hydrazine hydrates, suction filtration obtains product after 20min is stirred at room temperature.Then weigh suitable Bi
(NO3)3·5H2O, which is dissolved in 0.5mol/L nitric acid, is configured to 100ml, the aqueous solution of 0.01mol/L, is added and filters product ultrasound
20min is added dropwise ammonium hydroxide and is adjusted to pH value of reaction system 9, and magnetic agitation 0.5 hour is then washed with deionized water, ethyl alcohol successively,
Filtering, in the heating rate of 2 DEG C/min to 300 DEG C of roasting heat preservation 1h up to chemical composition after filter cake is dried 24 hours at 40 DEG C
For V2O5/BiVO4Vanadic anhydride/pucherite nano composite antibiotic material.
The characterization of the nano combined sterilization material of vanadic anhydride/pucherite：
X-ray diffraction analysis is the result shows that contain only V in composite material2O5And BiVO4Two-phase (Fig. 2).Pass through energy disperse spectroscopy
(EDS) it analyzes, as a result V in nano composite antibiotic material2O5/BiVO4Molar ratio be 0.62.
Embodiment 3
By NH4VO3Be configured to the aqueous solution of a concentration of 0.06mol/L, be added dropwise 2mL, in 1mol/L hydrochloric acid to system, after by
It is added dropwise to 12mL, 80% hydrazine hydrate, suction filtration obtains product after 40min is stirred at room temperature.Then weigh suitable Bi (NO3)3·5H2O
It is dissolved in 2mol/L nitric acid and is configured to 100ml, the aqueous solution of 0.02mol/L is added and filters product ultrasound 40min, and ammonium hydroxide is added dropwise
It is adjusted to pH value of reaction system 10, magnetic agitation 2 hours is then washed with deionized water, ethyl alcohol successively, filtering, by filter cake 50
In the heating rate of 10 DEG C/min to 500 DEG C of roasting heat preservation 5h up to chemical composition it is V DEG C after dry 24 hours2O5/BiVO4's
Vanadic anhydride/pucherite nano composite antibiotic material.
The characterization of the nano combined sterilization material of vanadic anhydride/pucherite：
X-ray diffraction analysis is the result shows that contain only V in composite material2O5And BiVO4Two-phase (Fig. 3), passes through energy disperse spectroscopy
(EDS) it analyzes, the results showed that V in nano composite antibiotic material2O5/BiVO4Molar ratio be 0.32.
Comparative example 1
Nano composite antibiotic material is prepared according to the method for embodiment 2, it is different to be：By NH4VO3It is configured to a concentration of
1mL is added dropwise in the aqueous solution of 0.08mol/L, in 2.5mol/L hydrochloric acid to system, after be added dropwise 6mL, 90 volume % hydrazine hydrates,
Suction filtration obtains product after 30min is stirred at room temperature.Then weigh suitable Bi (NO3)3·5H2O, which is dissolved in 1mol/L nitric acid, to be configured to
The aqueous solution of 100ml, 0.025mol/L.
Anti-biotic material characterization obtained：X-ray diffraction analysis is the result shows that there is BiVO in composite material4And Bi2O3(Fig. 4),
It is analyzed by energy disperse spectroscopy (EDS), the results showed that BiVO in nano composite antibiotic material4/Bi2O3Molar ratio be 3.8.
Comparative example 2
Nano composite antibiotic material is prepared according to the method for embodiment 2, it is different to be：
By filter cake at 70 DEG C after dry 26 hours in the heating rate of 15 DEG C/min in 550 DEG C of roasting heat preservation 6h up to chemistry
Group becomes V2O5/BiVO4Vanadic anhydride/pucherite nano composite antibiotic material.
Anti-biotic material characterization obtained：X-ray diffraction analysis is the result shows that contain only V in composite material2O5And BiVO4Two
Phase (Fig. 5) is analyzed, the results showed that V in nano composite antibiotic material by energy disperse spectroscopy (EDS)2O5/BiVO4Molar ratio be
0.65。
Test example 1
Anti-microbial property detects
It is 1.0mg/mL by photochemical catalyst dosage by anti-biotic material made from embodiment 1, it is black before carrying out illumination experiment
Dark 30min, measure respectively later illumination 30min, 60min and 120min and no light continue dark 30min, 60min and
120min materials are to the killing effect of pseudomonas aeruginosa (being purchased from ATCC, preserving number is ATCC 27853), bacteria technology
Using plate technique method, the results are shown in Figure 6.
Even if as can be seen from Figure 6 nano composite antibiotic material of the invention still has good under non-illuminated conditions
Bactericidal property, in the case where there is illumination condition, sterilization rate faster, can effectively solve the inorganic sterilization material of traditional photocatalysis unglazed
Without the technical barrier that bactericidal property or bactericidal property are weak according under the conditions of.
Test example 2
Embodiment 2, comparative example 1-2 and BiVO in the prior art4Photocatalysis antibacterial material (the limited public affairs of Shanghai WWRC Group chemical industry
Department, article No. CAS No.14059-33-7), it is used for antibacterial, as a result as described in Table 1.
Table 1
As can be seen from the above Table 1, the nano composite antibiotic material for preparation being reacted under the Parameter Conditions of the application has
Preferably composite bactericidal performance, compared to the anti-biotic materials prepared of comparative example 1-2 not under this condition in dark and sunshine
Under the conditions of bactericidal property be intended to height, wherein the anti-biotic material of comparative example 2 is than the bactericidal property of the anti-biotic material of comparative example 1
It is good, illustrate in the reaction process of the present invention particular solution match when concentration under, the better performances of sterilization material obtained,
And these parameters are affected to the performance of the anti-biotic material of preparation；And the dry anti-biotic material under the drying condition of the present invention
Bactericidal property it is preferable, but influence of the drying condition to sterilization material performance is relatively small；And embodiment 2, comparative example 1-2 systems
The bactericidal properties of standby anti-biotic material are above anti-biotic material in the prior art.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (5)
1. a kind of preparation method of nano composite antibiotic material, includes the following steps：
1）Hydrochloric acid is added dropwise to NH4VO3It in solution, is then added dropwise in hydrazine hydrate solution again, after being stirred at room temperature, suction filtration obtains
Reaction product；
2）Then the reaction product is added to Bi (NO3)3×5H2Ultrasonic mixing in O solution, then ammonium hydroxide is added dropwise and is adjusted to react
The pH value of system is alkalinity, obtains reaction mixture, then the reaction mixture is stirred to react, obtains filter cake；
3）Again will after the filtration cakes torrefaction, roast to get；
In step 1）In, by 0.5 ~ 2.0mL, 0.5 ~ 2.0mol/L hydrochloric acid is added dropwise to the NH of 0.03 ~ 0.06mol/L4VO3In solution,
Then it is added dropwise 4 ~ 12mL again, in the hydrazine hydrate solution of 80 volume %, 20 ~ 40min is stirred at room temperature, suction filtration obtains reaction product；
In step 2）In, the reaction product is added to 100mL, the Bi (NO of 0.001 ~ 0.02mol/L3)3×5H2In O solution
The pH value 9 ~ 10 that ammonium hydroxide is adjusted to reaction system is added dropwise in ultrasonic 20 ~ 40min of mixing, obtains reaction mixture, then the reaction is mixed
It closes object and stirs 0.5 ~ 2h, obtain filter cake.
2. the preparation method of nano composite antibiotic material according to claim 1, which is characterized in that by 1mL, 1mol/L salt
Acid is added dropwise to the NH of 0.05mol/L4VO3In solution, it is then added dropwise 6mL again, in the hydrazine hydrate solution of 80 volume %, room temperature is stirred
30min is mixed, suction filtration obtains reaction product.
3. the preparation method of nano composite antibiotic material according to claim 1, which is characterized in that by 100mL,
Bi (the NO of 0.005mol/L3)3×5H2Ultrasonic mixing 30min in the reaction product is added in O solution, and ammonium hydroxide is added dropwise and is adjusted to react
The pH value 10 of system obtains reaction mixture, then the reaction mixture is stirred to react 1 hour, obtains filter cake.
4. the preparation method of nano composite antibiotic material according to claim 1, which is characterized in that in step 3）In, institute
Filter cake is stated after 40 ~ 60 DEG C 24 hours dry, under the heating rate of 2 ~ 10 DEG C/min, is warming up to 300 ~ 500 DEG C of roasting heat preservations 1
~5 h。
5. the preparation method of nano composite antibiotic material according to claim 4, which is characterized in that the filter cake is in 60 DEG C
After 24 hours dry, under the heating rate of 5 DEG C/min, it is warming up to 400 DEG C of 2 h of roasting heat preservation.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4251283A (en) * | 1978-10-06 | 1981-02-17 | Montedison S.P.A. | Bismuth vanadate pigments and process for preparing same |
| CN103908960A (en) * | 2013-11-15 | 2014-07-09 | 大连理工大学 | Preparation method of V2O5/BiVO4 (vanadium pentoxide/bismuth vanadium oxide) nanorod composite photocatalyst |
-
2016
- 2016-01-25 CN CN201610049313.5A patent/CN105707122B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4251283A (en) * | 1978-10-06 | 1981-02-17 | Montedison S.P.A. | Bismuth vanadate pigments and process for preparing same |
| CN103908960A (en) * | 2013-11-15 | 2014-07-09 | 大连理工大学 | Preparation method of V2O5/BiVO4 (vanadium pentoxide/bismuth vanadium oxide) nanorod composite photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| Macroporous V2O5-BiVO4 Composites: Effect of Heterojunction on the Behavior of Photogenerated Charges;Juan Su et al;《The Journal of Physical Chemistry C》;20110405;第115卷(第6期);第8064-8071页 * |
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