CN107020055A - A kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials - Google Patents

A kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials Download PDF

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CN107020055A
CN107020055A CN201710435016.9A CN201710435016A CN107020055A CN 107020055 A CN107020055 A CN 107020055A CN 201710435016 A CN201710435016 A CN 201710435016A CN 107020055 A CN107020055 A CN 107020055A
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sio
zno
bead
polypody
shell structure
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CN107020055B (en
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冒国兵
刘琪
周贝贝
刘荣梅
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Anhui Polytechnic University
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    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • C02F1/00—Treatment of water, waste water, or sewage
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    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention discloses a kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials, methods described is by SiO2Bead surface growth in situ ZnO crystal seeds, the Ultrasonic Pulverization in growth solution, then obtains SiO through standing separation, washing and after drying afterwards2@ZnO core shell structure polypody bead nano composite materials.Using ultrasonic grind, using in situ synthesis, preparation condition is gentle, and technique is simple, is adapted to large area production.SiO prepared by the present invention2@ZnO core shell structure polypody beads composite gauge is uniform, and favorable dispersibility, composition is controllable, is expected to be applied in terms of photoelectric material or catalysis material.

Description

A kind of SiO2The preparation method of@ZnO core shell structure polypody bead nano composite materials and It is applied
Technical field
The invention belongs to nano combined new material technology field, and in particular to a kind of SiO2@ZnO core shell structure polypody beads The preparation method and applications of nano composite material.
Background technology
ZnO is a kind of typical broad stopband direct band-gap semicondictor material, is pacified with good biocompatibility and environment Quan Xing, in recent years as a kind of very promising catalysis material by the extensive concern of vast researcher.Many institute's weeks Know, the factor such as structure, pattern, surface state of photochemical catalyst directly affects its performance and application.By to preparation technology and bar The control of part, obtains the ZnO nano material of sizes and pattern, substantially increases its photocatalytic activity.ZnO nano material There is the defects such as nano-sized materials are easily reunited, quantum yield poor to organic matter absorption property is relatively low in actual applications, this It is a little to greatly limit raising and its application that ZnO light urges activity.Based on this, some ZnO/ heterojunction semiconductor composite woods are occurred in that Material, its preparation method is generally hydrothermal/solvent heat.As SiO2 and ZnO are combined, its structure is generally simple nano-particle or with ZnO For core, SiO2 colloids be hull shape into spherical nanoparticle.After SiO2 and ZnO is compound, some performances such as photoluminescence performance is obtained Raising is arrived.The hot method of hydrothermal/solvent needs closed high temperature and high pressure environment, is not suitable for large area production.Ultrasonic Pulverization prepares material Material is easy, quick, be adapted to prepared by large area the advantages of.ZnO nanorod, but its composite wood can occasionally be obtained using Ultrasonic Pulverization at present All there is bigger difficulty in preparation and separation in material.
The content of the invention
It is contemplated that at least solving one of technical problem present in prior art.Therefore, the present invention provides a kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials, it is therefore an objective to pass through simple, condition temperature The preparation technology of sum, obtains the nano composite material for improving photocatalytic activity.
To achieve these goals, the technical scheme taken of the present invention is：
A kind of SiO2The preparation method of@ZnO core shell structure polypody bead nano composite materials, methods described be by SiO2Bead surface growth in situ ZnO crystal seeds, the Ultrasonic Pulverization in growth solution afterwards, then through standing separation, washing and dry SiO is obtained after dry2@ZnO core shell structure polypody bead nano composite materials.
The preparation method of the present invention specifically includes following steps：
Step one, by electronegative SiO2Bead is added in the ZnO seed-solutions of positively charged, is obtained after vibration filtering SiO with ZnO crystal seeds2Bead；
Step 2, by the SiO with ZnO crystal seeds2Bead is added to the mixed aqueous solution of hexa and zinc nitrate In；
Step 3, by the SiO with ZnO crystal seeds2The mixed aqueous solution of bead Ultrasonic Pulverization under the conditions of 60-80 DEG C, it SiO is obtained by standing separation, washing and after drying2@ZnO core shell structure polypody beads.
The SiO2Bead surface growth in situ ZnO crystal seeds are by electronegative SiO2The ZnO that bead is added to positively charged is brilliant Plant in solution, the SiO with ZnO crystal seeds is obtained after vibration filtering2Bead.SiO2Bead surface is obtained by electrostatic adsorption ZnO crystal seeds are obtained, are easy to both to adsorb combination, and method is simply efficient.
The SiO2Bead and the mass concentration ratio of ZnO seed-solutions are 0.01g:0.2-1.0g/L.It is dense by this quality The addition of proportioning is spent, the SiO that form preferably carries ZnO crystal seeds is resulted in2Bead, SiO2The ZnO crystal seeds distribution of bead surface It is more uniform.If seed concentration is too low, SiO2The ZnO nanorod of bead surface growth is rare, does not become core shell structure；If Seed concentration is too high, SiO2The ZnO nanorod of bead surface growth easily comes off.
Growth solution is easy to the life of core shell structure polypody bead using hexa and the mixed aqueous solution of zinc nitrate Into, and it is not likely to produce other interference impurity.Zinc nitrate can be Zn (NO3)2●6H2O。
The mol ratio of the hexa and zinc nitrate is 1:1.Using the growth solution of this mol ratio, it is easy to SiO2The generation of@ZnO core shell structure polypody beads, grain crystalline is good.
The molar concentration of the hexa and zinc nitrate is 0.5-1.0mmol/L.Using this molar concentration scope It is easy to obtain the good SiO of form2@ZnO core shell structure polypody beads.
The temperature of Ultrasonic Pulverization is 60-80 DEG C in growth solution, and the time of Ultrasonic Pulverization is 1-4h.Crush temperature too It is low, SiO2Bead surface is difficult to growing ZnO nanorod；Grinding time is less than 1h, and the reaction time is short in solution, ZnO nanorod life Long incomplete, form is irregular；Reactive material in 4h or so solution exhausts substantially, reaction terminating.
The present invention is with business SiO2Bead is core, and ZnO nanorod is deposited on its surface, obtains SiO2@ZnO core shell structures are more Sufficient bead nano composite material.Polypody bead nanostructured cause its in the solution stably dispersing do not allow free settling, and particle Do not reunite between particle, reduce the contact between nanometer rods, increase the reactivity site in catalytic reaction, so that Its photocatalytic activity is obtained to improve.
Beneficial effects of the present invention：
(1) ultrasonic grind is used, using in situ synthesis, preparation condition is gentle, and technique is simple, is adapted to large area life Production；
(2) the new SiO that preparation method of the present invention is obtained2@ZnO core shell structure polypody bead nano composite materials are increased Reactivity site in catalytic reaction, improves photocatalytic activity.
(3) SiO prepared by the present invention2@ZnO core shell structure polypody beads composite gauge is uniform, favorable dispersibility, into Divide controllable.
(4) the new SiO that preparation method of the present invention is obtained2@ZnO core shell structure polypody bead nano composite materials, in gas The field such as absorption and catalysis of organic matter has big application potential in body or sewage or waste water.
Brief description of the drawings
This specification includes the following drawings, and shown content is respectively：
Fig. 1 is the XRD of product prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figures of product prepared by the embodiment of the present invention 1；
Wherein (a) SiO2Bead, (b) carries the SiO of ZnO crystal seeds2Bead, SiO prepared by (c) (d)2@ZnO core shell structures Polypody bead；
Fig. 3 is the SEM figures of product prepared by the embodiment of the present invention 2；The wherein SEM for the sample that (a) is obtained；(b) it is single SiO2The SEM figures of@ZnO core shell structure beads；
Fig. 4 is the SEM figures of product prepared by the embodiment of the present invention 3；The wherein SEM for the sample that (a) is obtained；(b) it is single SiO2The SEM figures of@ZnO core shell structure beads；
Fig. 5 is the SEM figures of product prepared by the embodiment of the present invention 4；
Fig. 6 is the SEM figures of product prepared by the embodiment of the present invention 5；
Fig. 7 is the SEM figures of the product of comparative example 1 of the present invention；
Fig. 8 is the SEM figures of the product of comparative example 2 of the present invention.
Embodiment
Below against accompanying drawing, by the description to embodiment, the embodiment to the present invention makees further details of Explanation, it is therefore an objective to help those skilled in the art to have more complete, accurate and deep reason to design of the invention, technical scheme Solution, and contribute to it to implement.
The present invention provides a kind of SiO2The preparation method of@ZnO core shell structure polypody beads, this method is by SiO2It is small Ball surface growth in situ ZnO crystal seeds, the Ultrasonic Pulverization in growth solution, is then obtained through standing separation, washing and after drying afterwards To SiO2@ZnO core shell structure polypody beads.
It is described in detail below by specific embodiment.
Embodiment 1
(1) first by 0.01g SiO2Bead is added in 0.5g/L ZnO seed-solutions to vibrate and filtered after 24h, obtains band There is the SiO of ZnO crystal seeds2Bead；
(2) 20mL 0.625mmol/L hexas (HMT) and 20mL 0.625mmol/L zinc nitrates is taken to prepare mixed Heshui solution, by the above-mentioned SiO with ZnO crystal seeds2Bead is added in above-mentioned mixed aqueous solution；
(3) above-mentioned mixed solution is put on electric furnace and heated, the temperature for making mixed liquor is 70 DEG C, and ultrasonic disintegrator is popped one's head in It is put into mixed solution, after Ultrasonic Pulverization 4h, separates, washs and dry by standing sedimentation, obtain SiO2@ZnO nucleocapsid knots Structure polypody bead nano composite material.
Product is analyzed using X-ray optical diffraction (XRD) and SEM (SEM).
Reference picture 1, sets forth the SiO with ZnO crystal seeds of the preparation of embodiment 12Bead and SiO2@ZnO composites XRD, for the ease of contrast, also give commercial SiO2The XRD of bead.
As a result the ZnO containing crystallization in the present embodiment product is shown, and ZnO diffraction maximum is more sharp, illustrates what is prepared ZnO particle well-crystallized.
Fig. 2 is the SiO used in the product preparation process of embodiment 12Bead and obtain the SiO with crystal seed2Bead and system Standby SiO2The SEM figures of@ZnO core shell structure polypody beads.It can be seen that commercialization SiO2Bead surface is smooth, and size is equal Even, diameter is about 800nm.In ZnO seed-solutions after oscillation treatment, SiO2Bead surface is roughened, and many attachments occurs in surface Particle.
Embodiment 2
The present embodiment and the difference of embodiment 1 are：The concentration of ZnO crystal seeds is 0.2g/L.Obtained product and reality Apply that example 1 is basically identical, only because the solubility of crystal seed is smaller, SiO2ZnO nanorod is not fine and close on bead, and it scans electron microscope As shown in Figure 3.(a) is the SEM figures of the sample prepared in Fig. 3, from the figure, it can be seen that having SiO simultaneously in sample2@ZnO Core-shell structure particles and ZnO nanorod, both are difficult to separate, so can see substantial amounts of ZnO nanorod simultaneously in figure. (b) it is a SiO in the sample2The SEM figures of@ZnO core-shell structure particles, it can be seen that obvious ZnO is brilliant from this particle Plant particle, SiO2Bead surface ZnO nanorod size is uneven.
Embodiment 3
The present embodiment and the difference of embodiment 1 are：The concentration of ZnO crystal seeds is 1.0g/L.Obtained product and reality Apply that example 1 is basically identical, it is as shown in Figure 4 that it scans electron microscope.Wherein (a) is the SEM figures of the sample prepared, and (b) is single SiO2@ The SEM figures of ZnO core-shell structure particles.From (a) as can be seen that the sample prepared is by uniform SiO2@ZnO core-shell structure particles groups Into not finding ZnO nanorod substantially；From (b) as can be seen that SiO2Surface is all covered by ZnO nanorod, is formd complete SiO2@ZnO core shell structures.
Embodiment 4
The present embodiment and the difference of embodiment 1 are：Zinc nitrate is Zn (NO3)2●6H2O, Zn (NO3)2●6H2O and The molar concentration of hexa is 0.5mol/L.
Product made from the present embodiment and embodiment 1 are basically identical, and zinc oxide foot ear of maize diameter is somewhat tiny, and it scans electricity Mirror figure is as shown in Figure 5.
Embodiment 5
The present embodiment and the difference of embodiment 1 are：Zinc nitrate is Zn (NO3)2●6H2O, Zn (NO3)2●6H2O, Zn(NO3)2●6H2O and hexa molar concentration 1.0mol/L.
Product made from the present embodiment and embodiment 1 are basically identical, and zinc oxide foot ear of maize diameter is thick, and it scans electron microscope As shown in Figure 6.
Comparative example 1
The present embodiment and the difference of embodiment 1 are：Prepare SiO2During@ZnO core shell structures, SiO2Bead without The processing of ZnO crystal seeds.
The SEM spectrograms of the present embodiment product are shown in Fig. 7.It can be seen that the product is by SiO2Ball and ZnO nanorod group Into.
Comparative example 2
The present embodiment and the difference of embodiment 1 are：Mixed solution is put on electric furnace and heated, makes the temperature of mixed liquor Spend for 80 DEG C, do not use after Ultrasonic Pulverization, reaction 2h, by sedimentation separation, wash and dry.The scanning electron microscopic picture of the product As shown in figure 8, SiO2The substantially not long upper ZnO nanorod of bead surface, only some ZnO crystal seed nano particles.
The present invention is exemplarily described above in association with accompanying drawing.Obviously, the present invention is implemented not by above-mentioned side The limitation of formula.As long as employ the improvement of the various unsubstantialities of inventive concept and technical scheme of the present invention progress；Or not It is improved, the above-mentioned design of the present invention and technical scheme are directly applied into other occasions, in protection scope of the present invention Within.

Claims (8)

1. a kind of SiO2The preparation method of@ZnO core shell structure polypody bead nano composite materials, it is characterised in that methods described is By in SiO2Bead surface growth in situ ZnO crystal seeds, the Ultrasonic Pulverization in growth solution afterwards, then through standing separation, wash Wash and obtain SiO after drying2@ZnO core shell structure polypody bead nano composite materials.
2. SiO according to claim 12The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the SiO2Bead surface growth in situ ZnO crystal seeds are by electronegative SiO2The ZnO crystal seeds that bead is added to positively charged are molten In liquid, the SiO with ZnO crystal seeds is obtained after vibration filtering2Bead.
3. SiO according to claim 22The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the SiO2Bead and the mass concentration ratio of ZnO seed-solutions are 0.01g:0.2-1.0g/L.
4. SiO according to claim 12The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the growth solution is the mixed aqueous solution of hexa and zinc nitrate.
5. SiO according to claim 42The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the mol ratio of the hexa and zinc nitrate is 1:1.
6. SiO according to claim 42The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the molar concentration of the hexa and zinc nitrate is 0.5-1.0mmol/L.
7. SiO according to claim 12The preparation method of@ZnO core shell structure polypody bead nano composite materials, its feature exists In the temperature of Ultrasonic Pulverization is 60-80 DEG C in growth solution, and the time of Ultrasonic Pulverization is 1-4h.
8. any one of the claim 1-7 SiO2@ZnO core shell structure polypody beads organic matter in gas, sewage or waste water Application in absorption.
CN201710435016.9A 2017-06-10 2017-06-10 SiO (silicon dioxide)2Preparation method and application of @ ZnO core-shell structure multi-legged pellet nanocomposite Expired - Fee Related CN107020055B (en)

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CN109428065A (en) * 2017-08-28 2019-03-05 内蒙古欣蒙碳纳米科技有限公司 A kind of preparation method of nanometer rods composite negative pole material
CN110124739A (en) * 2019-06-03 2019-08-16 江南大学 A kind of cross-linking type CD-MOF composite material and preparation method loading nano-photocatalyst
CN111659374A (en) * 2020-06-10 2020-09-15 江苏扬农化工集团有限公司 Catalyst, preparation method thereof and method for synthesizing hexamethylene diamine intermediate

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CN104549209A (en) * 2014-12-26 2015-04-29 哈尔滨工业大学 Double-faced zinc oxide nanoarray photocatalytic material and preparation method thereof
CN104907036A (en) * 2015-05-15 2015-09-16 燕山大学 Graded dandelion-flower-shaped ZnO-Al2O3 compound and preparation method therefor
CN104961151A (en) * 2015-07-10 2015-10-07 中国科学院上海硅酸盐研究所 Dandelion-shaped composite oxide nanoparticle as well as preparation method and application thereof
CN105381802A (en) * 2015-12-23 2016-03-09 哈尔滨工业大学 Method for preparing dandelion-shaped Fe3O4@ZnO core-shell structure compound on basis of heterogeneous nucleation method and application

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CN109428065A (en) * 2017-08-28 2019-03-05 内蒙古欣蒙碳纳米科技有限公司 A kind of preparation method of nanometer rods composite negative pole material
CN110124739A (en) * 2019-06-03 2019-08-16 江南大学 A kind of cross-linking type CD-MOF composite material and preparation method loading nano-photocatalyst
CN111659374A (en) * 2020-06-10 2020-09-15 江苏扬农化工集团有限公司 Catalyst, preparation method thereof and method for synthesizing hexamethylene diamine intermediate
CN111659374B (en) * 2020-06-10 2023-07-14 江苏扬农化工集团有限公司 Catalyst, preparation method thereof and method for synthesizing hexamethylenediamine intermediate

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