CN104910901A - Method used for preparing ZnO/SiO2 nano composite material - Google Patents
Method used for preparing ZnO/SiO2 nano composite material Download PDFInfo
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- CN104910901A CN104910901A CN201510272215.3A CN201510272215A CN104910901A CN 104910901 A CN104910901 A CN 104910901A CN 201510272215 A CN201510272215 A CN 201510272215A CN 104910901 A CN104910901 A CN 104910901A
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- zno
- composite material
- nano composite
- bromoacetic acid
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Abstract
The invention discloses a method used for preparing a ZnO/SiO2 nano composite material. The method comprises following steps: (1) produced zinc bromoacetic acid is dissolved in a mixed solution of water and ethanol so as to obtain a zinc bromoacetic acid solution, a mixed solution of TEOS which is taken as a silicon source and APTES which is used for providing amino group is dissolved in absolute ethyl alcohol, an obtained mixture is added into the zinc bromoacetic acid solution dropwise, and reaction is carried out for 4 to 6h; (2) an obtained product is subjected to centrifugation, is washed with ethanol for 2 to 3 times, and is subjected to drying in a vacuum oven so as to obtain a white powder; and (3) the white powder is delivered into a muffle furnace for roasting so as to obtain the ZnO/SiO2 nano composite material. According to the method, amino group in APTES is taken as a catalyst, silicon dioxide is obtained via catalysis of the silicon source, silicon dioxide particles are generated in roasting at last, no extra catalyst is needed in the reaction process, and the method is harmless for the environment, and is a green synthetic method.
Description
Technical field
The invention belongs to nano-composite mate-rial technical field, relate to a kind of making ZnO/SiO
2the method of nano composite material, is specifically related to a kind of autocatalysis hydrolytic sol gel method and generates ZnO/SiO
2the method of the nano composite material of fluorescent characteristic.
Background technology
In recent years, due to the special performance of zinc oxide, for it as the synthesis of nano material and the more and more extensive of functional study.Especially as should the having of nano composite material of nucleocapsid structure, the characteristic of ZnO can effectively be increased.As the shell material of clading ZnO, there are high molecular polymer, carbon material and silicon-dioxide available at present.But due to relations such as the thermostability of high molecular polymer and the intensity of carbon material, be subject to certain restrictions as in shell material use.Silicon-dioxide has thermostability, nontoxicity, the well transparency, meanwhile, silica sphere is easy to modify different functional groups, there is good biocompatibility, effectively can improve the surface imperfection of ZnO, improving its stability and consistency, is the optimal selection as ZnO nano shell material.A lot of researcher is attempted with various method synthesis ZnO/SiO
2nano combined material material.
In now a variety of methods, be all first be prepared into nano-ZnO mostly, ZnO surface being carried out modification increases and SiO
2consistency, finally add silicon source hydrolytic condensation again and realize SiO
2be coated on the outside of ZnO nanoparticle, or adopt the method for atom transfer, inside the particle of silicon-dioxide, synthesize ZnO, thus realize coated object.Above method, all also exist long reaction time, complex steps, cost high, to deficiencies such as the infringement of environment are large.
Summary of the invention
In order to solve complex steps in synthesizing nano compound material process in the past, cost is high, the time is long, deficiency to aspects such as bad environmental, the invention provides making ZnO/SiO that a kind of reaction conditions is gentle, the time is short, step is easy
2the method of nano composite material.
The object of the invention is to be achieved through the following technical solutions:
A kind of making ZnO/SiO
2the method of nano composite material, comprises the steps:
(1) ZnO and bromoacetic acid reaction generate bromoacetic acid zinc as presoma;
(2) the bromoacetic acid zinc of generation is dissolved in (volume ratio=1:1 of water and ethanol) in the mixed solution of water and ethanol, using as silicon source tetraethoxy (TEOS) and provide amino 3-aminopropyl triethoxysilane (APTES) mixed solution to be dissolved in dehydrated alcohol and be added drop-wise in the solution of bromoacetic acid zinc, controlling three's amount of substance than being bromoacetic acid zinc: APTES:TEOS=0.5 ~ 1.5:1 ~ 2:0.1 ~ 0.2, reacting 4 ~ 6 hours;
(3) gained material will be reacted centrifugal, by washing with alcohol 2 ~ 3 times, next dry in vacuum drying oven, obtain white powder;
(4) gained white powder is put into retort furnace to calcine, obtain ZnO/SiO
2nano composite material.
In above-mentioned reaction, the amount of described ZnO and bromoacetic acid is than being 1:2.
In above-mentioned reaction, described drying temperature is normal temperature, and time of drying is 20 ~ 30h.
In above-mentioned reaction, described centrifugal speed is 8000 ~ 10000r/min.
In above-mentioned reaction, described calcining temperature is 600 ~ 700 DEG C, and calcination time is 2 ~ 3 hours.
Add amino and silicon source in above-mentioned reaction on same material, the amino ion of the former release catalysis the latter can be hydrolyzed generation SiO
2, complete both and combine.Relative to other silicon source and amino, need not add organosilane and ammoniacal liquor, the present invention has the following advantages:
1, the bromoacetic acid zinc that the present invention is used is a kind of organic metal salt, does not damage environment, is a kind of Green Chemistry material;
2, the present invention utilizes amino contained in APTES to generate silicon-dioxide as catalyst silicon source, in the end also has silicon dioxide granule to generate in calcining, need not add other catalyzer in reaction process;
3, in method, silicon source and amino are same materials, can greatly reduce organic usage quantity, make reaction more succinct.
4, environmental sound in this reaction, belongs to green synthesis method.
Accompanying drawing explanation
Fig. 1 is ZnO/SiO
2the TEM image of nano composite material;
Fig. 2 is ZnO/SiO
2with bromoacetic acid zinc/SiO
2infrared image;
Fig. 3 is ZnO/SiO
2fluorescent spectrum curve.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1
One, the preparation of bromoacetic acid zinc: 1g ZnO and 3.415g bromoacetic acid are put into the single necked round bottom flask that 100ml high purity water is housed successively, react 1h under 60 DEG C of conditions, filters and obtains settled solution, with Rotary Evaporators, solvent evaporated away is obtained white solid.
Two, ZnO/SiO
2the preparation of fluorescence nano composite material: the bromoacetic acid zinc of 1.4g is dissolved in (volume ratio=1:1 of water and ethanol) in the mixing solutions of 60ml water and ethanol.The tetraethoxy mixed solution of 2.17ml 3-aminopropyl triethoxysilane and 0.17ml is dissolved in the dehydrated alcohol of 40ml and is added drop-wise in the solution of bromoacetic acid zinc, control three's amount of substance than being bromoacetic acid zinc: APTES:TEOS=1:2:0.15, normal temperature and pressure lower magnetic force stirs 6h, centrifugal, speed is 8500r/min, obtains white powder after removing supernatant liquid.Following dehydrated alcohol repetitive scrubbing 2 ~ 3 times, the dry 24h of vacuum drying oven, calcines 1.5h and removes organism under 650 DEG C of conditions.Silicon in the 3-aminopropyl triethoxysilane that early stage adds changes generation silicon-dioxide, and generates ZnO nano particle, finally makes ZnO/SiO
2fluorescence nano composite material, its pattern as shown in Figure 1.
In Fig. 2, a is after drying, the white powder infrared image before calcining, and b is the image of gained material after calcining.As can be seen from figure, we, eliminate corresponding organo-functional group and structure before calcination afterwards, remained inorganic Zn-O key and Si-O key, illustrate generate material inside have these two kinds of materials of ZnO and SiO2.
As shown in Figure 3, the material obtained after calcining, under the exciting of 350nm UV-light, creates fluorescence phenomenon.
Embodiment 2
One, the preparation of 3-bromo-propionic acid zinc: 1g ZnO and 4.2g 3-bromo-propionic acid have been joined in 100ml high purity water single necked round bottom flask successively, after 60 DEG C of water-bath 1.5h, gained solution is filtered, the settled solution obtained is evaporated solvent completely under Rotary Evaporators, obtains white powder.
Two, ZnO/SiO
2the preparation of fluorescence nano composite material, in the mixed solution being 1:1 by water-soluble for 1.5g 3-bromo-propionic acid zinc and ethanol contend ratio.2.1ml APETS and 0.2mlTEOS mixed solution being joined in the 3-bromo-propionic acid zinc solution being added drop-wise in 40ml dehydrated alcohol and by this and previously having obtained, controlling three's amount of substance than being bromoacetic acid zinc: APTES:TEOS=1:2:0.15.React 6h under normal temperature and pressure, centrifugal, speed 8000r/min, by washing with alcohol 2-3 time.Air drying 24h in vacuum drying oven, puts into retort furnace at 650 DEG C of calcining 2h, the organic group in removing white powder by dry for gained white powder.After cooling, finally obtain ZnO/SiO
2fluorescence nano composite material.
Claims (7)
1. making ZnO/SiO
2the method of nano composite material, is characterized in that described method steps is as follows:
(1) the bromoacetic acid zinc of generation is dissolved in the mixed solution of water and ethanol, using as silicon source TEOS and provide amino APTES mixed solution to be dissolved in dehydrated alcohol and be added drop-wise in the solution of bromoacetic acid zinc, controlling three's amount of substance than being bromoacetic acid zinc: APTES:TEOS=0.5 ~ 1.5:1 ~ 2:0.1 ~ 0.2, reacting 4 ~ 6 hours;
(2) gained material will be reacted centrifugal, by washing with alcohol 2 ~ 3 times, next dry in vacuum drying oven, obtain white powder;
(3) gained white powder is put into retort furnace to calcine, obtain ZnO/SiO
2nano composite material.
2. making ZnO/SiO according to claim 1
2the method of nano composite material, is characterized in that described bromoacetic acid zinc is reacted by ZnO and bromoacetic acid and generates.
3. making ZnO/SiO according to claim 2
2the method of nano composite material, is characterized in that the amount of described ZnO and bromoacetic acid than being 1:2.
4. making ZnO/SiO according to claim 1
2the method of nano composite material, is characterized in that in the mixed solution of described water and ethanol, the volume ratio=1:1 of water and ethanol.
5. making ZnO/SiO according to claim 1
2the method of nano composite material, it is characterized in that described drying temperature is normal temperature, time of drying is 20 ~ 30h.
6. making ZnO/SiO according to claim 1
2the method of nano composite material, is characterized in that described centrifugal speed is 8000 ~ 10000r/min.
7. making ZnO/SiO according to claim 1
2the method of nano composite material, it is characterized in that described calcining temperature is 600 ~ 700 DEG C, calcination time is 2 ~ 3 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880873A (en) * | 2017-11-06 | 2018-04-06 | 郑州大学 | Zinc oxide barium sulfate composite nano materials preparation method, zinc oxide barium sulfate composite nano materials, application and LED chip |
| CN109232987A (en) * | 2017-07-11 | 2019-01-18 | 上海曦灵化工科技有限公司 | A kind of preparation method of silicon dioxide carried nanocomposite and plastic master batch |
| CN113979466A (en) * | 2021-10-27 | 2022-01-28 | 烟台佳隆纳米产业有限公司 | ZnO@SiO2Preparation method of nano capsule |
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| CN101942300A (en) * | 2009-07-09 | 2011-01-12 | 中国科学院理化技术研究所 | Granular ZnO/SiO with adjustable refractive index2Luminescent composite material and its preparation method and use |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232987A (en) * | 2017-07-11 | 2019-01-18 | 上海曦灵化工科技有限公司 | A kind of preparation method of silicon dioxide carried nanocomposite and plastic master batch |
| CN109232987B (en) * | 2017-07-11 | 2021-02-05 | 上海曦灵化工科技有限公司 | Preparation method of silicon dioxide loaded nano composite material and plastic master batch |
| CN107880873A (en) * | 2017-11-06 | 2018-04-06 | 郑州大学 | Zinc oxide barium sulfate composite nano materials preparation method, zinc oxide barium sulfate composite nano materials, application and LED chip |
| CN113979466A (en) * | 2021-10-27 | 2022-01-28 | 烟台佳隆纳米产业有限公司 | ZnO@SiO2Preparation method of nano capsule |
| CN113979466B (en) * | 2021-10-27 | 2023-04-28 | 烟台佳隆纳米产业有限公司 | ZnO@SiO 2 Method for preparing nanocapsules |
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Application publication date: 20150916 |