CN106477620A - A kind of preparation method of the transparent alcoholic solution of nano zine oxide - Google Patents
A kind of preparation method of the transparent alcoholic solution of nano zine oxide Download PDFInfo
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The present invention relates to a kind of preparation method of the transparent alcoholic solution of nano zine oxide, comprises the following steps：(1) NaOH is added in ethanol and mixes, it is sufficiently stirred for, obtain sodium hydroxide solution, (2) zinc salt is added in ethanol and mixes, it is sufficiently stirred for, polyethylene glycol is added, then stirring obtains zinc solution, (3) sodium hydroxide solution is quickly adding in zinc solution, continues stirring reaction at 48～52 DEG C and obtain nano zine oxide ethanol solution in 20～800 minutes.The present invention has the advantage that：(1) the ultra-fine ZnO@PEG nano particle of scale controllable standby, ethanol solution good stability, can keep clear more than 6 months, and occur nothing particle agglomeration phenomenon.(2) after the ethanol solution of the nano zine oxide has more stable photoluminescent property, and 6 days, can still retain 91.0% fluorescence intensity, also there is after the ethanol solution dilute with water of the nano particle certain stability.
Description
Technical field
The present invention relates to a kind of preparation method of the transparent alcoholic solution of nano zine oxide, belongs to field of inorganic nonmetallic material.
Background technology
In the past few years, Zinc oxide nanoparticle receives extensive research, and especially in transparent conductor, photoelectricity turns
Change, Industrial Catalysis, the field such as biological medicine.Compared with Cd system and Pb system fluorescence quantum, zinc oxide has nontoxic and biofacies
The features such as capacitive, it is particularly suitable for biomedicine field.When the particle diameter of solid particle is less than certain characteristic length scales（As swashed
Sub- diameter or electron mean free path）When, its physics and chemistry attribute differs markedly from intrinsic bulk material, especially zinc oxide nanocrystalline
Body.Compared with titanium dioxide nano-particle, nano zine oxide is experimentally easier to realize quantum confined effect.Therefore, study
The method for preparing super fine zinc oxide nano particle with exploitation scale is significant.Up to the present, with regard to superfine nano
The definition of particle is the presence of dispute.Recently, it has been proposed that the main standard divided as superfine nano particle using 10 nm.
Additionally, also including for defining the dimension of superfine nano particle：Sub- 10 nm grain sizes, nano SiO 2 particle, gold nano
Particle；5 nm grain sizes, CdSe, gold, silver, copper, nano-sized iron oxide.Up to the present, scientific worker employs various each
The method synthesizing superfine Zinc oxide nanoparticle of sample, such as ultraviolet light decomposition method, microreactor-film dispersion method, polyethyleneimine-wet
Chemical method, organic metal method for hydrolysis etc..However, these synthetic methods often encounter problems with：As superfine nano oxidation
Zinc particles stability is poor, syntheti c route complicated, synthesis cost is too high.Between 20 years of past, synthesizing zinc oxide in ethanol
Nano particle is widely studied：The nucleation of nano zine oxide and growth mechanism, the stabilization of smaller ligand, nano oxygen
Change the stability regular of zinc colloidal sol.However, few people's research stability of the zinc oxide nano-particle by high polymer modification after with
Fluorescent characteristic.By the stable nano-particle of high polymer be regulate and control in colloidal dispersion system between nano particle interactive effectively
One of method.There is obvious advantage using high polymer stable nanoparticles：The stability of nano particle is difficult by solution ring
Border (there is electrolyte, water/non-water environment) and the impact of particle concentration.Therefore, by zinc-oxide nano that high polymer is stable
The bioluminescence application of grain may be more suitable for the biotic environment of complexity.
Chinese invention patent 201310428767.X is disclosed《A kind of method for preparing monodisperse spherical nano ZnO》,
Which is with zinc salt, NaOH and PEG-6000 as raw material, prepares, using one-step method, the spherical nano-ZnO that particle diameter is about 30nm.
The nano-ZnO footpath grain that the method is prepared is larger（About 30nm）, and ethanol dispersion of the nano-ZnO insoluble in alcohol, i.e. nano-ZnO
Property is poor.At present, the pertinent literature report of high ethano dispersiveness and the good nano zine oxide preparation method of fluorescence property there are no.
Content of the invention
The technical problem to be solved in the present invention is：A kind of preparation method of the transparent alcoholic solution of nano zine oxide, the party are provided
It is zinc source that method selects zinc salt, and NaOH is alkali source, and polyethylene glycol is stabilizer, in ethanol low-temp reaction, and nano oxygen is obtained
Change zinc ethanol solution；Within obtained nano zine oxide average grain diameter can be controlled in 5nm, with the dispersed and fluorescence of high ethano
Can be good.
Solve above-mentioned technical problem technical scheme be：A kind of preparation method of the transparent alcoholic solution of nano zine oxide, including
Following steps：
(1) NaOH is added in ethanol and mixes, NaOH and ethanol mol ratio are 0.001～0.006,48
It is sufficiently stirred at～52 DEG C 18～22 minutes, sodium hydroxide solution is obtained,
(2) zinc salt is added in ethanol and mixes, zinc salt is 0.001～0.006,63～68 DEG C with the mol ratio of ethanol
Under be sufficiently stirred for 18～22 minutes, be cooled to 48～52 DEG C, add in polyethylene glycol, the addition of polyethylene glycol and step (2)
The volume ratio of ethanol consumption is 1～7:100, then stir 8～12 minutes at 48～52 DEG C, obtain zinc solution；
(3) sodium hydroxide solution is quickly adding in zinc solution, sodium hydroxide solution is 1 with the volume ratio of zinc solution：
1～1.1, continue stirring reaction 20～800 minutes at 48～52 DEG C, obtain nano zine oxide ethanol solution.
In step (2), described zinc salt is zinc acetate, the one kind in zinc chloride, zinc sulfate, two or three.
In step (2), described polyethylene glycol is polyethylene glycol -200, PEG-4000, PEG-400
A kind of, two or three.
Due to employing above technical scheme, the invention has the advantages that：
(1) the ultra-fine ZnO@PEG nano particle of scale controllable standby.The ethanol solution good stability of the nano zine oxide, 6
Holding clear state that can be stable in the time of more than individual month, and occur nothing particle agglomeration phenomenon, as shown in Figure 7.
(2), after the ethanol solution of the nano zine oxide has more stable photoluminescent property, and 6 days, can still retain
91.0% fluorescence intensity, as shown in Figure 6.After the ethanol solution dilute with water of the nano particle, its fluorescence also has certain steady
Qualitative.
Description of the drawings
Fig. 1 is the saturating of the ZnO@PEG nano particle of acquisition in nano zine oxide ethanol solution prepared by the embodiment of the present invention 1
Penetrate electron microscope picture spectrum（TME）.The zinc oxide dispersion that can be seen that present invention preparation from the projection electron microscope of Fig. 1 is equal
Even, particle diameter is 5nm or so.
Fig. 2 is the transmission electron microscope figure spectrum of unmodified ZnO nano particle（TME）.
Fig. 3 is the ZnO@PEG nano particle and not obtained in nano zine oxide ethanol solution prepared by the embodiment of the present invention 1
Fourier's infared spectrum of modification ZnO nano particle（FTIR）.In figure, A are ZnO@PEG nano particle, and B is received for unmodified ZnO
Rice grain.From figure 3, it can be seen that due to the stretching vibration of Zn-O key, unmodified ZnO nano particle and ZnO@PEG nano particle
In 460 cm-1All there is strong vibration absorption peak in place.For ZnO@PEG nano particle, due to polyethylene glycol bag
The presence of thing is wrapped up in, in 1250 cm-1Place ,-C-O-H in-plane bending vibration peak can be found, meanwhile, in 1100 cm-1Place ,-C-
O (H) stretching vibration peak is also found.However, the two peaks do not find the FT-IR absorption spectra in unmodified ZnO nano particle
In, the result fully shows, polyethylene glycol can adsorb in ZnO@PEG nanoparticle surface.
Fig. 4-1 is the thermogravimetric collection of illustrative plates of unmodified ZnO nano particle（TGA）.Fig. 4-2 is receiving for the preparation of the embodiment of the present invention 1
The thermogravimetric collection of illustrative plates of the ZnO PEG nano particle obtained in rice zinc oxide ethanol solution（TGA）.Can from Fig. 4-1 and Fig. 4-2
Go out, weightless through three steps, the total weight-loss ratio of ZnO@PEG nano-particle is 62%, and total weight-loss ratio of unmodified ZnO nanoparticle is
36.25%.Additionally, for unmodified ZnO nanoparticle, at 120 DEG C, its weight loss rate reaches maximum（0.375 %/
℃）, and ZnO@PEG nano-particle will can be only achieved maximum by weight loss rate at 250 DEG C, and maximum weight loss rate is only 0.55
%/℃.Can it is conjectured that：Unmodified ZnO nanoparticle and ZnO@PEG nano-particle maximum weight loss rate are respectively by unmodified
In ZnO sample, in volatile solvent and ZnO@PEG sample, the thermal decomposition of polyethylene glycol polymer chain causes.Therefore, TGA analysis knot
Fruit further demonstrates that：During ZnO@PEG nano-particle is prepared, its particle surface is wrapped up by polyethylene glycol polymer.
Fig. 5 is the X ray diffracting spectrum of unmodified ZnO nano particle（XRD）.From fig. 5, it can be seen that it is obvious that
31.60 °, 34.318 °, 36.08 ° can be found diffraction maximum, correspond respectively to (1 1 0) of wurtzite-type zinc oxide, (0 0
2), (1 0 1) crystal face.Above-mentioned all results fully show that polyethylene glycol can adsorb in ZnO@PEG nano grain surface, and
Reciprocation is produced with which.
Fig. 6：ZnO@PEG ethanol solution is in 4 DEG C of storages fluorescent stability figure of 6 days.From fig. 6, it can be seen that its fluorescence spoke
Penetrate that intensity can retain initial intensity 91.0%, shows：In ethanol, ZnO@PEG nano particle occupies acceptable storage
Stability, can be used in the fluorescence sense analysis of correlation.In addition the result is verified further：Polyethylene glycol can effectively prevent oxygen
Change zinc nanoparticles reunion in ethanol, the Lacking oxygen compound on its surface can be protected, and ZnO PEG nano particle is accounted for
According to excellent fluorescence sense performance.
Fig. 7：Nano zine oxide ethanol solution and unmodified nano-ZnO ethanol solution pair prepared by the embodiment of the present invention 1
Than figure.From figure 7 it can be seen that after the ethanol solution of unmodified Zinc oxide nanoparticle stores 24 h at room temperature, its ethanol
Solution turned cloudy and a large amount of zinc oxide precipitate are can be found that in holding bottle bottom.However, at ambient temperature, prepared by the present invention
The ethanol solution of ZnO@PEG nano particle stable transparent can be kept to reach 6 months.
In Fig. 7, a is one day unmodified nano-ZnO ethanol solution of storage, and b is the storage nano-ZnO@of the present invention of 6 months
PEG ethanol solution.
Specific embodiment
Embodiment 1:
10.0 mmol NaOH are dissolved in 100.0 mL ethanol（Equivalent to 1.7mol ethanol）, stir 20 minutes at 50 DEG C, make
Sodium hydroxide solution.Meanwhile, 10.0 mmol Zn (AC)2·2H2O is dissolved in 100.0 mL ethanol, stirring 20 minutes at 65 DEG C, so
After be cooled to 50 DEG C, add 5.0 mL PEG-200, at 50 DEG C stir 10 minutes, make acetic acid zinc solution.Finally, will
100.0mL sodium hydroxide solution is rapidly added in 101.0mL acetic acid zinc solution, continues 20～800 points of stirring reaction at 50 DEG C
Clock, obtains transparent nano-zinc oxide ethanol solution.
The nano zine oxide ethanol solution that the differential responses time is obtained is put and is preserved in 4 DEG C.In order to obtain through poly- second
The Zinc oxide nanoparticle of glycol modification, adds 200 mL distilled water, so in the obtained nano zine oxide ethanol solution of reaction
It is centrifuged 5 minutes under 4000 turns/min afterwards, topples over supernatant liquor, precipitation alcohol flushing 3 times, at 40 DEG C, then dry 48
H, is obtained ZnO@PEG nano particle, and for carrying out the sign such as FT-IR, TGA, XRD.In the case of without PEG 200,
Unmodified Zinc oxide nanoparticle is prepared according to above-mentioned identical method.
Embodiment 2:
10.0 mmol NaOH are dissolved in 100.0 mL ethanol, are stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0 mmol zinc acetates are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 1.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes acetic acid zinc solution.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL acetic acid zinc solution, at 50 DEG C, continue stirring reaction 20 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 3:
10.0 mmol NaOH are dissolved in 100.0 mL ethanol, are stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0 mmol zinc acetates are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 3.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes acetic acid zinc solution.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL acetic acid zinc solution, at 50 DEG C, continue stirring reaction 40 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 4:
10.0 mmol NaOH are dissolved in 100.0 mL ethanol, are stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0 mmol zinc acetates are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 5.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes acetic acid zinc solution.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL acetic acid zinc solution, at 50 DEG C, continue stirring reaction 60 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 5:
10.0 mmol NaOH are dissolved in 100.0 mL ethanol, are stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0 mmol zinc acetates are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 7.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes acetic acid zinc solution.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL acetic acid zinc solution, at 50 DEG C, continue stirring reaction 80 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 6:
10.0mmol NaOH is dissolved in 100.0 mL ethanol, is stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0mmol zinc chloride is dissolved in 100.0 mL ethanol, stirs 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, adds 5.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes liquor zinci chloridi.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL liquor zinci chloridi, at 50 DEG C, continue stirring reaction 120 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 7:
10.0mmol NaOH is dissolved in 100.0 mL ethanol, is stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 10.0 mmol zinc chloride are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 7.0
ML PEG-200, stirs 10 minutes at 50 DEG C, makes liquor zinci chloridi.Finally, 100.0mL sodium hydroxide solution is added rapidly
Enter in 101.0mL liquor zinci chloridi, at 50 DEG C, continue stirring reaction 200 minutes, transparent nano-zinc oxide ethanol solution is obtained,
And clear can be kept more than 6 months.
Embodiment 8：
10.0mmol NaOH is dissolved in 100.0 mL ethanol, is stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 5.0 mmol zinc sulfate are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 7.0 mL
PEG-200, stirs 10 minutes at 50 DEG C, makes solution of zinc sulfate.Finally, 100.0mL sodium hydroxide solution is rapidly added
In 101.0mL solution of zinc sulfate, at 50 DEG C, continue stirring reaction 200 minutes, transparent nano-zinc oxide ethanol solution is obtained, and
Clear can be kept more than 6 months.
Embodiment 9：
10.0mmol NaOH is dissolved in 100.0 mL ethanol, is stirred 20 minutes at 50 DEG C, makes sodium hydroxide solution.With
When, 5.5 mmol zinc sulfate are dissolved in 100.0 mL ethanol, stir 20 minutes, be subsequently cooled to 50 DEG C at 65 DEG C, add 7.0 mL
PEG-200, stirs 10 minutes at 50 DEG C, makes solution of zinc sulfate.Finally, 100.0mL sodium hydroxide solution is rapidly added
In 101.0mL solution of zinc sulfate, at 50 DEG C, continue stirring reaction 200 minutes, transparent nano-zinc oxide ethanol solution is obtained, and
Clear can be kept more than 6 months.
In various embodiments of the present invention, the ethanol for preparing sodium hydroxide solution and solution of zinc sulfate each means anhydrous second
Alcohol.
The present invention by the use of zinc acetate as zinc source, polyethylene glycol -200 as stabilizer, controlled be hydrolyzed-be crosslinked anti-
Should, synthesize ZnO@PEG nano particle ethanol solution.
In reaction system, add the polyethylene glycol constraint chain of polyethylene glycol, zinc oxide surface to occupy different conformations certainly
By spending.The macromolecular chain for occupying different conformational freedoms can interpenetrate, and to a certain extent, reduce inside wrappage and receive
The reunion free energy of rice grain so that nano particle can be stable in the presence of in respective media environment.
It is 800 minutes between when reacted, prepared nano zine oxide ethanol solution is still able to keep clarification.
Claims (3)
1. the preparation method of the transparent alcoholic solution of a kind of nano zine oxide, it is characterised in that：Comprise the following steps：
(1) NaOH is added in ethanol and mixes, NaOH and ethanol mol ratio are 0.001～0.006,48
It is sufficiently stirred at～52 DEG C 18～22 minutes, sodium hydroxide solution is obtained,
(2) zinc salt is added in ethanol and mixes, zinc salt is 0.001～0.006,63～68 DEG C with the mol ratio of ethanol
Under be sufficiently stirred for 18～22 minutes, be cooled to 48～52 DEG C, add in polyethylene glycol, the addition of polyethylene glycol and step (2)
The volume ratio of ethanol consumption is 1～7:100, then stir 8～12 minutes at 48～52 DEG C, obtain zinc solution；
(3) sodium hydroxide solution is quickly adding in zinc solution, sodium hydroxide solution is 1 with the volume ratio of zinc solution：
1～1.1, continue stirring reaction 20～800 minutes at 48～52 DEG C, obtain nano zine oxide ethanol solution.
2. the preparation method of the transparent alcoholic solution of a kind of nano zine oxide according to claim 1, it is characterised in that：Step
(2), in, described zinc salt is zinc acetate, the one kind in zinc chloride, zinc sulfate, two or three.
3. the preparation method of the transparent alcoholic solution of a kind of nano zine oxide according to claim 1 and 2, it is characterised in that：Step
Suddenly, in (2), described polyethylene glycol is polyethylene glycol -200, PEG-4000, one kind of PEG-400, two kinds or
Three kinds.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390282A (en) * | 2020-11-16 | 2021-02-23 | 郑州大学 | Hydrophilic zinc oxide quantum dot and preparation method and application thereof |
| CN114031973A (en) * | 2021-12-21 | 2022-02-11 | 上海永安印务有限公司 | High-adhesion water-based ink and preparation method thereof |
| CN116285960A (en) * | 2023-03-08 | 2023-06-23 | 郑州大学 | Preparation method of large-size transparent scintillator |
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| CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
| CN103145175A (en) * | 2013-03-14 | 2013-06-12 | 西安交通大学 | Preparation method of small-size nano-zinc oxide powder |
| CN103359774A (en) * | 2013-07-28 | 2013-10-23 | 桂林理工大学 | Preparation method of castor-oil-coated zinc oxide nano particle |
| CN103972395A (en) * | 2014-04-30 | 2014-08-06 | 深圳清华大学研究院 | Zinc oxide composite material, preparing method of zinc oxide composite material and solar cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
| CN103145175A (en) * | 2013-03-14 | 2013-06-12 | 西安交通大学 | Preparation method of small-size nano-zinc oxide powder |
| CN103359774A (en) * | 2013-07-28 | 2013-10-23 | 桂林理工大学 | Preparation method of castor-oil-coated zinc oxide nano particle |
| CN103972395A (en) * | 2014-04-30 | 2014-08-06 | 深圳清华大学研究院 | Zinc oxide composite material, preparing method of zinc oxide composite material and solar cell |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390282A (en) * | 2020-11-16 | 2021-02-23 | 郑州大学 | Hydrophilic zinc oxide quantum dot and preparation method and application thereof |
| CN114031973A (en) * | 2021-12-21 | 2022-02-11 | 上海永安印务有限公司 | High-adhesion water-based ink and preparation method thereof |
| CN114031973B (en) * | 2021-12-21 | 2022-09-30 | 上海永安印务有限公司 | High-adhesion water-based ink and preparation method thereof |
| CN116285960A (en) * | 2023-03-08 | 2023-06-23 | 郑州大学 | Preparation method of large-size transparent scintillator |
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