CN106477621A - Stratiform zinc hydroxide, the preparation of zinc-oxide nano cone and stripping means - Google Patents
Stratiform zinc hydroxide, the preparation of zinc-oxide nano cone and stripping means Download PDFInfo
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- CN106477621A CN106477621A CN201610917575.9A CN201610917575A CN106477621A CN 106477621 A CN106477621 A CN 106477621A CN 201610917575 A CN201610917575 A CN 201610917575A CN 106477621 A CN106477621 A CN 106477621A
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
The invention discloses a kind of preparation of stratiform zinc hydroxide, zinc-oxide nano cone and stripping means.It is that the mixing of metal zinc salt, alkali source and anionic surfactant is carried out heating in water bath in pure aquatic system, reaction obtains the homogeneous stratiform zinc hydroxide nanocone of pattern.Stratiform zinc hydroxide nanocone is placed in heating in reaction system peel off, obtains monolayer zinc hydroxide nanometer sheet, stratiform zinc hydroxide nanocone is obtained porous zinc bloom nanocone by high-temperature calcination simultaneously.The present invention has the advantages that process is simple, safe operation, the suitability are wide, overcomes the particle size heterogeneity that existing synthetic route prepares, building-up process uncontrollable and the problems such as cost power consumption is higher.Using the product novel in shape of present invention preparation, size uniformity, and there is good layer structure, in Adsorption of Organic, the aspect such as photocatalysis has broad application prospects.
Description
Technical field
The invention belongs to field of material preparation is and in particular to stratiform zinc hydroxide, the preparation of zinc-oxide nano cone and stripping
From method.
Background technology
It is known that stratified nano materials are as the important component part of inorganic non-metallic function nano material, its main body
It is usually that interact the two-dimensional nanostructure material piled up, wherein, plate are passed through by two kinds of metallic elements and interlayer ion
Atom within layer is to be combined with each other by covalent bond or hydrogen bond, and interlayer is by weak Van der Waals force or electrostatic interaction and mainboard
Layer is connected.Therefore it is also called bimetallic layered hydroxide, referred to as (LDHs), its chemical composition formula is：M1-x 2+Nx 3+
(OH)2Ax/n n-·mH2O.In 20 end of the centurys, even if it was discovered by researchers that in the presence of there is no trivalent metallic element, according to
So the stratified material with hydrotalcite-like compound can be formed, its chemical composition is usually：M(OH)2-xAx/n n-·mH2O, referred to as α
The layered hydroxide of phase.The stratified material that these have hydrotalcite-like compound is a class novel inorganic functional material, because of its tool
There is abundant interlayer ion to exchange and peelable characteristic, have broad application prospects in optics, electro-catalysis field.Bond material
Itself and construction featuress, the methods having been developed in multiple synthesis layered hydroxides in recent years, also prepare different-shape simultaneously
The laminar nano particle of feature.The forerunner that Yusuke Yamauchi et al. will be synthesized by the use of high molecular polymer as directed agents
Body has simultaneously obtained stratiform Ni (OH) by the calcining of different temperatures2Nano flower (Chem.Commum., 2012,48,9150-
9152).S.Jin et al. reports and is successfully prepared Co-Ni layered hydroxide using the continuous hydrothermal solution reaction of High Temperature High Pressure
(Nano.Lett.,2015,15,1421-1427).X.H.Liu et al. is successfully prepared stratiform hydroxide using microwave heating method
Cobalt nanocone (Adv.Mater., 2012,24,2148-2153).However, synthesizing the method for layered hydroxide at present still more
Complexity, power consumption is more, and the synthesis of stratiform zinc hydroxide nano material is very few with stripping research.Therefore, develop a kind of simple to operate,
The preparation method of the stratified nano materials of energy-conserving and environment-protective is a vital task of field of material preparation.
Content of the invention
Object of the present invention is to provide a kind of simple to operate, energy-conserving and environment-protective and the controlled stratiform hydroxide of technological process
The synthesis of zinc and zinc-oxide nano cone and stripping means.
A kind of stratiform zinc hydroxide, the preparation method of nanocone, comprise the following steps：
Step 1：By metal zinc salt, alkali source, and/or anion surfactant in the system with pure water as reaction dissolvent
Mixing；
Step 2：The mixing liquid heating in water bath for reaction of step 1 is obtained stratiform zinc hydroxide or zinc oxide.
Metal zinc salt described in step 1 be zinc chloride or zinc nitrate, alkali source be hexamethylenetetramine, carbamide, ammonia or
Sodium hydroxide；Anionic surfactant is sodium lauryl sulphate.
Metal zinc salt described in step 1 is 1 with the mol ratio of anion surfactant:0.8～2.5, alkali source with cloudy from
The mol ratio of sub- surfactant is：8.75:1～3.125, the molal quantity of alkali source and the volume ratio of pure water are 1mmol:15-
20mL.
Metal zinc salt described in step 1 is preferably 1 with the mol ratio of anion surfactant:2.5, alkali source and anion
The mol ratio of surfactant is preferably 8.75:3.125, the molal quantity of alkali source and the volume ratio of pure water are preferably 1mmol:
17mL.
80～95 DEG C of water bath heating temperature in step 2,4～8 hours response time.Further preferably it is warming up at 95 DEG C anti-
Answer 8h.
The preparation method of porous zinc bloom nanocone, takes the stratiform zinc hydroxide nanometer that above-mentioned preparation method prepares
Cone proceeds in porcelain boat, and high-temperature calcination generates porous ZnO nanocone.High-temperature calcination is to be to slowly warm up to 700～1000 DEG C, insulation
0.5～4h.Preferably slow heating rate is 1 DEG C/min, is warming up to 800 DEG C and is incubated 0.5～4h.Further preferably it is warming up to
800 DEG C and be incubated 2h.
The stripping means of the stratiform zinc hydroxide nanocone that the present invention prepares：The stratiform that said method is prepared
Zinc hydroxide nanocone proceeds to and fills Methanamide and pure water (both volume ratios 1:4), in the there-necked flask mixing, oil bath heating arrives
80～90 DEG C of reaction 2～12h.Further preferably at 80 DEG C of temperature, peel off 8h and obtain monolayer zinc hydroxide nanometer sheet.
The present invention, compared with present technology, specifically has the advantage that and salience effect：
1st, adopt water-bath as course of reaction, can more effectively control course of reaction, save energy is it is possible to well
Expand reaction system, improve yield.
2nd, adopt the water-bath of suitable temperature as reaction condition, the good consumption of control surface activating agent and alkali source
Select, the stratiform zinc hydroxide nanometer sheet of different-shape, nano belt, nanocone, and zinc oxide nano rod, nanometer can be obtained
Granule etc., is shown in the embodiment of the present invention.
3rd, the present invention adopts common metal zinc salt as raw material, using pure water as reaction dissolvent；The anionic surface adding
Activating agent serves not only as interlayer intercalating ions in the forming process of stratiform zinc hydroxide nanocone, plays surfactant simultaneously
Effect.
4th, the present invention have studied different alkali sources to the thing phase of synthetic and the impact of shape characteristic, and finds alkali source
(hexamethylenetetramine) and sodium lauryl sulphate collective effect obtain stratiform zinc hydroxide nanocone.
5th, the present invention adopts the method stripped laminar zinc hydroxide nanocone of oil bath heating, and obtains the zinc hydroxide of monolayer
Nanometer sheet it should be noted that：Nanometer sheet thickness is about 0.9nm.
6th, using the stratiform zinc hydroxide nanocone that synthesizes as precursor, directly proceed to the calcining of magnetic boat high temperature is the present invention
Porous ZnO nanocone can be prepared.
7th, the present invention is pollution-free, and products obtained therefrom quality is high, and yield is controlled, has at the aspect such as photocatalytic degradation and fluorescence radiation
Extensively apply.
Brief description
Fig. 1 is the X-ray powder diffraction figure of the stratiform zinc hydroxide nanocone prepared by embodiment 1；
Fig. 2 is the SEM Electronic Speculum detection figure of the stratiform zinc hydroxide nanocone prepared by embodiment 1；
Fig. 3 is the high power SEM Electronic Speculum detection figure of the stratiform zinc hydroxide nanocone prepared by embodiment 1；
Fig. 4 is TEM Electronic Speculum detection figure and the SAED collection of illustrative plates of the stratiform zinc hydroxide nanocone prepared by embodiment 1；
Fig. 5 is the SEM Electronic Speculum detection figure of the zinc oxide nano rod prepared by embodiment 2；
Fig. 6 is the SEM Electronic Speculum detection figure of the stratiform zinc hydroxide nanometer sheet prepared by embodiment 3；
Fig. 7 be embodiment 4 prepared by stratiform zinc hydroxide nanocone, nanometer sheet SEM Electronic Speculum detection figure；
Fig. 8 is that the X of the stratiform zinc hydroxide nano belt, nanometer sheet and zinc-oxide nano prepared by embodiment 5,6,7 penetrates
Line powder diagram；
Fig. 9 is the SEM Electronic Speculum detection figure of the stratiform zinc hydroxide nano belt prepared by embodiment 5；
Figure 10 is the SEM Electronic Speculum detection figure of the stratiform zinc hydroxide nanometer sheet prepared by embodiment 6；
Figure 11 is the SEM Electronic Speculum detection figure of the Zinc oxide nanoparticle prepared by embodiment 7；
Figure 12 is the AFM Electronic Speculum detection figure of the monolayer zinc hydroxide nanometer sheet prepared by embodiment 8；
Figure 13 is the TEM Electronic Speculum detection figure of the monolayer zinc hydroxide nanometer sheet prepared by embodiment 8；
Figure 14 is the X-ray powder diffraction figure of the zinc-oxide nano cone prepared by embodiment 9；
Figure 15 is the SEM Electronic Speculum detection figure of the porous zinc bloom nanocone prepared by embodiment 9；
Figure 16 is the high power SEM Electronic Speculum detection figure of the porous zinc bloom nanocone prepared by embodiment 9；
Figure 17 is the TEM Electronic Speculum detection figure of the porous zinc bloom nanocone prepared by embodiment 9, SAED and HRTEM Electronic Speculum
Detection figure.
Specific embodiment
Following examples are intended to further illustrate the present invention, and the unrestricted present invention.
Embodiment 1
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 3.125mmol
(0.9g) sodium lauryl sulphate is dissolved in pure water, adds the hexa-methylene of 8.75mmol (1.225g) after uniform stirring 10min
Tetramine, seals up beaker mouth with preservative film after continuing stirring 15min, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.Will
React the product that obtains be centrifuged, wash, be dried after obtain white powder.Product is through X-ray powder diffraction as shown in Figure 1
It is accredited as stratiform zinc hydroxide；With scanning electron microscope (SEM), morphology analysis are carried out to stratiform zinc hydroxide, can from Fig. 2,3
Go out the nanocone that its pattern is about 1.5 μm for length；Carry out pattern with transmission electron microscope (TEM) to stratiform zinc hydroxide to divide
Analysis, as can be seen from Figure 4 its pattern is the nanocone of stratiform.
Embodiment 2
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, add after uniform stirring 10min
Enter the hexamethylenetetramine of 8.75mmol (1.225g), seal up beaker mouth with preservative film after continuing stirring 15min, beaker is moved
Enter in 95 DEG C of water-baths, be incubated 8 hours.White powder is obtained after the product that obtains of reaction is centrifuged, washs, being dried.
With scanning electron microscope (SEM), morphology analysis are carried out to it, as can be seen from Figure 5 its pattern is zinc oxide nano rod.
Embodiment 3
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 1mmol
(0.288g) sodium lauryl sulphate is dissolved in pure water, adds six methylenes of 8.75mmol (1.225g) after uniform stirring 10min
Urotropine, seals up beaker mouth with preservative film after continuing stirring 15min, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.
White powder is obtained after the product that obtains of reaction is centrifuged, washs, being dried.With scanning electron microscope (SEM), shape is carried out to it
Looks are analyzed, and as can be seen from Figure 6 its pattern is stratiform zinc hydroxide nanometer sheet.
Embodiment 4
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 2mmol
(0.476g) sodium lauryl sulphate is dissolved in pure water, adds six methylenes of 8.75mmol (1.225g) after uniform stirring 10min
Urotropine, seals up beaker mouth with preservative film after continuing stirring 15min, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.
White powder is obtained after the product that obtains of reaction is centrifuged, washs, being dried.With scanning electron microscope (SEM), shape is carried out to it
Looks are analyzed, and as can be seen from Figure 7 its pattern is stratiform zinc hydroxide nanometer sheet and nanocone.
Embodiment 5
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 3.175mmol
(0.9g) sodium lauryl sulphate is dissolved in pure water, adds the carbamide of 8.75mmol (0.525g) after uniform stirring 10min, continues
Seal up beaker mouth with preservative film after stirring 15min, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.Reaction is obtained
Product is centrifuged, washs, be dried after obtain white powder.Product is accredited as stratiform through X-ray powder diffraction as shown in Figure 8
Zinc hydroxide；With scanning electron microscope (SEM), morphology analysis are carried out to it, as can be seen from Figure 9 its pattern is stratiform zinc hydroxide
Nano belt.
Embodiment 6
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 3.175mmol
(0.9g) sodium lauryl sulphate is dissolved in pure water, adds a certain amount of ammonia after uniform stirring 10min, continues stirring 15min
Seal up beaker mouth with preservative film afterwards, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.By the product that obtains of reaction through from
The heart separate, washing, be dried after obtain white powder.Product is accredited as stratiform hydroxide through X-ray powder diffraction as shown in Figure 8
Zinc；With scanning electron microscope (SEM), morphology analysis are carried out to it, it can be seen that its pattern is stratiform zinc hydroxide nanometer sheet from 10.
Embodiment 7
Weigh zinc chloride 1.25mmol (0.17g) to be dissolved in the beaker filling 150ml pure water, then weigh 3.175mmol
(0.9g) sodium lauryl sulphate is dissolved in pure water, adds the NaOH of 8.75mmol after uniform stirring 10min, continues stirring
Seal up beaker mouth with preservative film after 15min, beaker is moved in 95 DEG C of water-baths, is incubated 8 hours.The product that reaction is obtained
Be centrifuged, wash, be dried after obtain white powder.Product is accredited as zinc oxide through X-ray powder diffraction as shown in Figure 8；
With scanning electron microscope (SEM), morphology analysis are carried out to it, as can be seen from Figure 11 its pattern is Zinc oxide nanoparticle.
Embodiment 8
Stratiform zinc hydroxide nanocone 0.1g weighing synthesis proceeds in 250ml there-necked flask, measures stripping solution first
Amide and pure water, liquor capacity is than for 1：4 proceed in there-necked flask, are placed in oil bath and are heated with stirring to 80 DEG C, are incubated 8h.Will be anti-
The solution centrifugal that should obtain, takes supernatant, obtains monolayer zinc hydroxide nanometer sheet solution.Right using atomic force microscope (AFM)
The pattern of monolayer zinc hydroxide nanometer sheet and thickness are analyzed, as can be seen from Figure 12 zinc hydroxide be individual layer nanometer sheet and
Thickness is about 0.9nm；Morphology analysis are carried out to monolayer zinc hydroxide nanometer sheet using transmission electron microscope (TEM), from Figure 13
In it can be seen that product be zinc hydroxide nanometer sheet.
Embodiment 9
Stratiform zinc hydroxide nanocone 0.1g weighing synthesis proceeds in magnetic boat, is positioned in Muffle furnace, and Muffle furnace is with 1
DEG C/heating rate of min is warming up to 800 DEG C and is incubated 2h, obtains milky sample.Product is through x-ray powder as shown in figure 14
Diffraction is accredited as zinc oxide；With scanning electron microscope (SEM), morphology analysis are carried out to zinc oxide, can be seen that pattern from Figure 15,16
Zinc-oxide nano cone for porous；With transmission electron microscope (TEM), morphology analysis are carried out to zinc oxide, can from Figure 17
Going out its pattern is porous taper zinc oxide；And prove that synthetic is crystallinity further with reference to HRTEM picture and SAED collection of illustrative plates
Good zinc oxide.
Claims (10)
1. a kind of preparation method of stratiform zinc hydroxide nanocone is it is characterised in that comprise the following steps：
Step 1：Metal zinc salt, alkali source, and anion surfactant are mixed in the system with pure water as reaction dissolvent；
Step 2：The mixing liquid heating in water bath for reaction of step 1 is obtained.
2. preparation method according to claim 1 it is characterised in that the metal zinc salt described in step 1 be zinc chloride or
Zinc nitrate, alkali source is hexamethylenetetramine；Anionic surfactant is sodium lauryl sulphate.
3. preparation method according to claim 1 is it is characterised in that the metal zinc salt described in step 1 and anionic surface
The mol ratio of activating agent is 1:0.8～2.5, alkali source with the mol ratio of anion surfactant is：8.75:1～3.125, alkali
The molal quantity in source and the volume ratio of pure water are 1mmol:15-20mL.
4. preparation method according to claim 1 is it is characterised in that the metal zinc salt described in step 1 and anionic surface
The mol ratio of activating agent is preferably 1:2.5, alkali source is preferably 8.75 with the mol ratio of anion surfactant:3.125, alkali source
The volume ratio of molal quantity and pure water be preferably 1mmol:17mL.
5. preparation method according to claim 1 is it is characterised in that 80～95 DEG C of water bath heating temperature in step 2, reaction
4～8 hours time.Further preferably it is warming up to reaction 8h at 95 DEG C.
6. the preparation method of porous zinc bloom nanocone is it is characterised in that by the preparation method described in any one of claim 1-5
The stratiform zinc hydroxide nanocone materials preparing proceed in porcelain boat, and high-temperature calcination generates porous ZnO nanocone.
7. preparation method according to claim 6 is it is characterised in that high-temperature calcination is to be to slowly warm up to 700～1000 DEG C,
Insulation 0.5～4h.
8. preparation method according to claim 7, it is characterised in that slow heating rate is 1 DEG C/min, is warming up to 800
DEG C and be incubated 0.5～4h.
9. preparation method according to claim 8 is it is characterised in that being warming up to 800 DEG C and being incubated 2h.
10. the stripping means of stratiform zinc hydroxide nanocone is it is characterised in that by the preparation described in any one of claim 1-5
The stratiform zinc hydroxide nanocone that method prepares proceeds to and fills volume ratio 1:In 4 Methanamide and pure water mixed solvent, oil
Bath is heated to 80～90 DEG C of reaction 2～12h, obtains monolayer zinc hydroxide nanometer sheet；Further preferably oil bath heating is at 80 DEG C
Reaction 8h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107487789A (en) * | 2017-07-06 | 2017-12-19 | 中南大学 | A kind of stratiform nickel cobalt hydroxide nano pipe cone and its preparation method and application |
| CN107866212A (en) * | 2017-11-08 | 2018-04-03 | 吉林大学 | A kind of rectangular patch photocatalyst of zinc oxide, preparation method and its application in photocatalytic hydrogen production by water decomposition |
| CN108543530A (en) * | 2018-03-15 | 2018-09-18 | 中国科学技术大学先进技术研究院 | A kind of Zinc oxide nano sheet in oxygen-enriched vacancy, preparation method and applications |
| CN110526276A (en) * | 2019-08-19 | 2019-12-03 | 上海大学 | A kind of preparation method and its air-sensitive application of ultra-thin Zinc oxide nano sheet |
| US11139371B2 (en) | 2018-10-08 | 2021-10-05 | National Tsing Hua University | Two-dimensional semiconductor with geometry structure and generating method thereof |
| CN113788502A (en) * | 2021-08-17 | 2021-12-14 | 天津大学 | Material preparation and detection method for distinguishing phosphate ion concentration in water environment |
| DE102021210870A1 (en) | 2021-09-29 | 2023-03-30 | Robert Bosch Gesellschaft mit beschränkter Haftung | Micellar particle, method for its production and its use |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107487789A (en) * | 2017-07-06 | 2017-12-19 | 中南大学 | A kind of stratiform nickel cobalt hydroxide nano pipe cone and its preparation method and application |
| CN107487789B (en) * | 2017-07-06 | 2021-10-22 | 中南大学 | Layered nickel-cobalt hydroxide nanotube cone and preparation method and application thereof |
| CN107866212A (en) * | 2017-11-08 | 2018-04-03 | 吉林大学 | A kind of rectangular patch photocatalyst of zinc oxide, preparation method and its application in photocatalytic hydrogen production by water decomposition |
| CN107866212B (en) * | 2017-11-08 | 2020-04-10 | 吉林大学 | Rectangular flaky zinc oxide photocatalyst, preparation method and application thereof in hydrogen production through photocatalytic water decomposition |
| CN108543530A (en) * | 2018-03-15 | 2018-09-18 | 中国科学技术大学先进技术研究院 | A kind of Zinc oxide nano sheet in oxygen-enriched vacancy, preparation method and applications |
| CN108543530B (en) * | 2018-03-15 | 2021-07-27 | 中国科学技术大学先进技术研究院 | Zinc oxide nanosheet with oxygen-enriched vacancy as well as preparation method and application thereof |
| US11139371B2 (en) | 2018-10-08 | 2021-10-05 | National Tsing Hua University | Two-dimensional semiconductor with geometry structure and generating method thereof |
| CN110526276A (en) * | 2019-08-19 | 2019-12-03 | 上海大学 | A kind of preparation method and its air-sensitive application of ultra-thin Zinc oxide nano sheet |
| CN113788502A (en) * | 2021-08-17 | 2021-12-14 | 天津大学 | Material preparation and detection method for distinguishing phosphate ion concentration in water environment |
| CN113788502B (en) * | 2021-08-17 | 2023-02-17 | 天津大学 | Material preparation and detection method for distinguishing phosphate ion concentration in water environment |
| DE102021210870A1 (en) | 2021-09-29 | 2023-03-30 | Robert Bosch Gesellschaft mit beschränkter Haftung | Micellar particle, method for its production and its use |
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