CN101428857A - Inducement control synthesis of zinc molybdate nano-material - Google Patents
Inducement control synthesis of zinc molybdate nano-material Download PDFInfo
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- CN101428857A CN101428857A CNA2008102047026A CN200810204702A CN101428857A CN 101428857 A CN101428857 A CN 101428857A CN A2008102047026 A CNA2008102047026 A CN A2008102047026A CN 200810204702 A CN200810204702 A CN 200810204702A CN 101428857 A CN101428857 A CN 101428857A
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Abstract
The invention discloses a method for synthesizing zinc molybdate nano materials under the control of induction. The method comprises the following steps: weighing a zinc source, a molybdenum source and a topography control agent respectively; placing in a high-pressure autoclave with a polytetrafluoroethylene lining; adding a certain amount of distilled water; closing the high-pressure autoclave, placing the high-pressure autoclave in an oven and heating at 140 to 200 DEG C for 2 to 12 hours; gradient-cooling the high-pressure autoclave to the room temperature and taking out after the reaction; absorbing the supernatant liquor; placing the sediment product in a beaker; ultrasonic processing for 30 minutes; standing for 0.5 to 2 hours; centrifugalizing; then sequentially rinsing with distilled water, acetone and absolute alcohol respectively for 3 times to obtain the product of the invention; and finally, preserving the product in the absolute alcohol. The product is the lath-shaped (needle coke and granular) zinc molybdate nano material with superior optical and electrical properties. The invention has the advantages of easily accessible material, easy operation, low cost, environment friendliness, convenient instrument and equipment, mild reaction condition, easily controllable product topography and structure, and convenient industrialized production.
Description
Technical field
The present invention relates to a kind of inducement control synthesis of zinc molybdate nano-material.
Background technology
The zinc molybdate of black molybdenum ore structure has broad application prospects in industries such as optics, electronics, biology, coating, medicine, buildings owing to its unique physicochemical property, structural performance, the scintillator characteristics of luminescence etc.The requirement of photoelectric device microminiaturization press for obtain rich and varied, pattern is different, the zinc molybdate material of unique properties, this makes its synthetic preparation difficulty more simultaneously.Up to the present, only there is few scientists to be devoted to the preparation and the performance study thereof of zinc molybdate powder and crystalline material.The method for preparing at present zinc molybdate powder and crystalline material thereof has: high-temperature high-voltage reaction method, solid reaction process and the precipitator method.
Yet, above-mentioned first three plant reaction method and all have 600 ℃ of temperature of reaction height (〉 in various degree), the production cost height, produce toxic gas and the product pattern is difficult to problems such as control, large-scale production is very difficult.Therefore develop a kind of convenient and simple, with low cost, environmental protection, reaction conditions gentleness, can scale production zinc molybdate material method significant.
Summary of the invention
Technical problem to be solved by this invention provides the inducement control synthesis of a kind of with low cost, environmental protection, reaction conditions gentleness, the zinc molybdate nano-material that is produced on a large scale.
The technical solution used in the present invention
A kind of inducement control synthesis of zinc molybdate nano-material comprises the following steps:
(1) takes by weighing zinc source, molybdenum source and morphology control agent respectively, it is presented to has in the teflon-lined autoclave, in autoclave, add distilled water, make the volumetric molar concentration in zinc source and molybdenum source be respectively 0.3～1.0mol/L, 0.3～1.0mol/L, the morphology control agent concentration is 0～7g/L, seal autoclave then and be placed in the baking oven 140～200 ℃ of heating 2～12 hours, take out after after reaction finishes the autoclave gradient being chilled to room temperature;
Wherein zinc is selected from a kind of in zinc chloride, zinc nitrate or the zinc acetate of solubility, and described molybdenum source is selected from Na
2MoO
4, K
2MoO
4Or H
2MoO
4In a kind of.The morphology control agent is a kind of in nitrilotriacetic acid(NTA), hexadecyl-trimethylammonium bromide, citric acid, the Paraformaldehyde 96.
(2) with the supernatant liquid in the reactor with the sucking-off of glue head dropper, lower sediment places beaker, with supersound process 30 minutes, leave standstill 0.5～2 hour after, use the supercentrifuge centrifugation, rotating speed is controlled to be 4000r/min, the time is 10min;
(3) precipitated product that centrifugation is obtained cleans respectively three times with distilled water, acetone and dehydrated alcohol successively, can obtain product of the present invention.
Product is kept in the dehydrated alcohol.
In described zinc salt of step (1) and molybdenum source: adding 0.2g nitrilotriacetic acid(NTA), hexadecyl-trimethylammonium bromide, citric acid, Paraformaldehyde 96 all can be induced the end product zinc molybdate material of synthetic different-shape, and the fluorescence peak generation blue shift of product.
Adding 0.2g citric acid can obtain the needle coke shape end product zinc molybdate of long 8 μ m, wide 600nm, and the fluorescence peak generation blue shift of product;
Adding 0.2g nitrilotriacetic acid(NTA) can obtain the long slab strip end product zinc molybdate of long 4 μ m, wide 500nm, high 200nm, and the fluorescence peak generation blue shift of product;
Adding 0.2g hexadecyl-trimethylammonium bromide can obtain the wide plate strip end product zinc molybdate of long 1.5 μ m, wide 800nm, high 200nm, and the fluorescence peak generation blue shift of product;
Adding 0.2g Paraformaldehyde 96 can obtain being of a size of the particulate state end product zinc molybdate of 80nm, and obvious blue shift takes place the fluorescence peak of product.
Characterize with scanning radio sub-microscope (SEM) and X-ray powder diffraction (XRD) pattern and structure products therefrom of the present invention.
The beneficial effect of the invention, advantage of the present invention is as follows:
The present invention is that a kind of inducing by introducing morphology control agent in the hydro-thermal synthetic system synthesized the zinc molybdate material.As a kind of effective material synthesis method, the key distinction of hydrothermal method and traditional other wet chemical methods such as sol-gel method is temperature and pressure.This method is in special closed reactor (autoclave), by type of heating make the reactant aqueous solution system produce one in temperature (100～300 ℃), hyperbaric environment a kind of effective ways of carrying out inorganic synthetic and material preparation, but synthetic yield is up to 90% and have a ZnMoO of different-shape
4Material.The zinc molybdate nano-material of the present invention's preparation has performances such as good light, electricity, and absorption peak blue shift, fluorescence strengthen.
In this reaction system, simple hydrothermal system only can obtain the product of single size and pattern, but but can obtain the different product of multiple pattern by introducing the morphology control agent.The present invention selects zinc salt and molybdenum source to react in the hydro-thermal encloses container, adds the pattern of morphology control agent induced product, has obtained panoramic zinc molybdate material.In this reaction system, can wait product size and pattern and crystal structure degree by kind and concentration, the morphology control agent introducing of control reactant.
Raw material of the present invention is easy to get, and is with low cost, simple to operate, and plant and instrument is easy, product pattern and easy control of structure, and the purity height, it is convenient to handle, and is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is scanning electronic microscope (SEM) figure of embodiment 1 product;
Fig. 2 is X-ray powder diffraction (XRD) figure of embodiment 1 product;
Fig. 3 is the fluorescence spectrum figure of embodiment 1 product.
Embodiment
Below by drawings and Examples the present invention is described in further detail, but do not limit the present invention.
Used analytical instrument: scanning electronic microscope, x-ray diffractometer, spectrophotofluorometer.
Embodiment 1
(1) take by weighing respectively the zinc chloride of 0.010mol and potassium molybdate, 0.2g citric acid it is presented to have polytetrafluoroethyllining lining, volume is in the autoclave of 45mL, in autoclave, add 30mL distilled water, seal autoclave then and be placed in the baking oven 160 ℃ of heating 6 hours, take out after after reaction finishes the autoclave gradient being chilled to room temperature;
(2) with the supernatant liquid in the reactor with the sucking-off of glue head dropper, lower sediment places beaker, with supersound process 30 minutes, leave standstill 0.5 hour after, use the supercentrifuge centrifugation, rotating speed is controlled to be 4000r/min, the time is 10min;
(3) precipitated product that centrifugation is obtained cleans respectively three times with distilled water, acetone and dehydrated alcohol successively, can obtain product of the present invention, at last product is kept in the dehydrated alcohol.Characterize with scanning electronic microscope and x-ray powder diffraction instrument pattern and structure respectively product, as can be seen from Fig. 1, SEM shows that product is the zinc molybdate needle coke of long 8 μ m, wide 600nm, as can be seen from Fig. 2, XRD result shows that product is pure, and is consistent with polycrystalline diffraction data storehouse (JCPDS card).As can be seen from Fig. 3, fluorescent spectroscopy is the result show, product has photoluminescence performance, and blue shift appears in emission peak.
Embodiment 2
Take by weighing 0.020mol zinc sulfate and potassium molybdate, 0.2g hexadecyl-trimethylammonium bromide respectively, then it is transferred in the 45mL band teflon-lined autoclave, in 140 ℃ of heating 12 hours, time of repose was 2 hours.Other conditions and step and embodiment 1 are identical, and the product that obtains is the zinc molybdate wide lath of long 1.5 μ m, wide 800nm, high 200nm, and the crystallographic system of product is identical with embodiment 1.
Embodiment 3
Take by weighing 0.030mol zinc nitrate and Sodium orthomolybdate, 0.2g nitrilotriacetic acid(NTA) respectively, other conditions and step and embodiment 1 are identical, and the product that obtains is the ZnMoO of long 4 μ m, wide 500nm, high 200nm
4Long lath, the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are good.Compare with embodiment 1, the blue shift degree of fluorescence peak is bigger.
Embodiment 4
Take by weighing 0.010mol zinc acetate and Sodium orthomolybdate, 0.2g Paraformaldehyde 96 respectively in 200 ℃ of heating 4 hours, other conditions and step and embodiment 1 are identical, and the product that obtains is 80 to be of a size of the zinc molybdate nano particle of 50nm, and the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are basic similar to embodiment 1.
Embodiment 5
Take by weighing 0.010mol zinc chloride and Sodium orthomolybdate respectively, other conditions and step and embodiment 1 are identical, and the product that obtains is the zinc molybdate nano particle of 80nm, and the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are basic similar to embodiment 1.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (6)
1, a kind of inducement control synthesis of zinc molybdate nano-material is characterized in that comprising the following steps:
(1) takes by weighing zinc source, molybdenum source and morphology control agent respectively, it is presented to has in the teflon-lined autoclave, in autoclave, add distilled water, make the volumetric molar concentration in zinc source and molybdenum source be respectively 0.3～1.0mol/L, 0.3～1.0mol/L, the morphology control agent concentration is 0～7g/L, seal autoclave then and be placed in the baking oven 140～200 ℃ of heating 2～12 hours, take out after after reaction finishes the autoclave gradient being chilled to room temperature;
Wherein the zinc source is selected from a kind of in zinc chloride, zinc nitrate or the zinc acetate of solubility; The molybdenum source is selected from Na
2MoO
4, K
2MoO
4Or H
2MoO
4In a kind of; The morphology control agent is a kind of in nitrilotriacetic acid(NTA), hexadecyl-trimethylammonium bromide, citric acid, the Paraformaldehyde 96.
(2) with the supernatant liquid in the reactor with the sucking-off of glue head dropper, lower sediment places beaker, with supersound process 30 minutes, leave standstill 0.5～2 hour after, use the supercentrifuge centrifugation, rotating speed is controlled to be 4000r/min, the time is 10min;
(3) precipitated product that centrifugation is obtained cleans respectively three times with distilled water, acetone and dehydrated alcohol successively, can obtain product of the present invention.
2, according to the inducement control synthesis of the described zinc molybdate nano-material of claim 1, it is characterized in that: in inducement control synthesis step (1), add the 0.2g citric acid, can obtain the zinc molybdate needle coke of long 8 μ m, wide 600nm in step (3).
3, according to the inducement control synthesis of the described zinc molybdate nano-material of claim 1, it is characterized in that: in inducement control synthesis step (1), add 0.2g hexadecyl-trimethylammonium bromide, can obtain the zinc molybdate wide lath of long 1.5 μ m, wide 800nm, high 200nm in step (3).
4, according to the inducement control synthesis of the described zinc molybdate nano-material of claim 1, it is characterized in that: in inducement control synthesis step (1), add the 0.2g nitrilotriacetic acid(NTA), can obtain the zinc molybdate long lath of long 4 μ m, wide 500nm, high 200nm in step (3).
5, according to the inducement control synthesis of the described zinc molybdate nano-material of claim 1, it is characterized in that: in inducement control synthesis step (1), add the 0.2g Paraformaldehyde 96, can obtain being of a size of the zinc molybdate particle of 80nm in step (3).
6, the inducement control synthesis of zinc molybdate nano-material as claimed in claim 1 is characterized in that the fluorescence peak generation blue shift of the resulting zinc molybdate material of step (3).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717120B (en) * | 2009-12-14 | 2011-08-03 | 上海应用技术学院 | Solvent thermal induction control synthesis method for nano molybdate with scheelite structure |
| CN102267723A (en) * | 2011-06-26 | 2011-12-07 | 河北联合大学 | Method for synthesizing zinc molybdate nanosheet by virtue of a structure-directing-agent-assisted microwave radiation method |
| CN102502834A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods |
| CN103950981A (en) * | 2014-05-20 | 2014-07-30 | 西北有色金属研究院 | Preparation method of zinc molybdate micropowder |
| CN105540669A (en) * | 2015-12-07 | 2016-05-04 | 陕西科技大学 | Preparation method of zinc molybdate and application of zinc molybdate in lithium ion battery negative electrode material |
| CN106564950A (en) * | 2016-11-09 | 2017-04-19 | 陕西科技大学 | Magnesium molybdate/graphene nanosheet array and preparation method therefor |
| CN107739546A (en) * | 2017-10-31 | 2018-02-27 | 华东理工大学 | A kind of inorganic anti-corrosion pigment with molybdic acid zinc modification |
-
2008
- 2008-12-16 CN CN2008102047026A patent/CN101428857B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717120B (en) * | 2009-12-14 | 2011-08-03 | 上海应用技术学院 | Solvent thermal induction control synthesis method for nano molybdate with scheelite structure |
| CN102267723A (en) * | 2011-06-26 | 2011-12-07 | 河北联合大学 | Method for synthesizing zinc molybdate nanosheet by virtue of a structure-directing-agent-assisted microwave radiation method |
| CN102502834A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods |
| CN102502834B (en) * | 2011-11-07 | 2013-10-09 | 河北联合大学 | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods |
| CN103950981A (en) * | 2014-05-20 | 2014-07-30 | 西北有色金属研究院 | Preparation method of zinc molybdate micropowder |
| CN103950981B (en) * | 2014-05-20 | 2015-11-18 | 西北有色金属研究院 | A kind of preparation method of zinc molybdate micro mist |
| CN105540669A (en) * | 2015-12-07 | 2016-05-04 | 陕西科技大学 | Preparation method of zinc molybdate and application of zinc molybdate in lithium ion battery negative electrode material |
| CN106564950A (en) * | 2016-11-09 | 2017-04-19 | 陕西科技大学 | Magnesium molybdate/graphene nanosheet array and preparation method therefor |
| CN106564950B (en) * | 2016-11-09 | 2017-12-22 | 陕西科技大学 | A kind of magnesium molybdate/graphene nano chip arrays and preparation method thereof |
| CN107739546A (en) * | 2017-10-31 | 2018-02-27 | 华东理工大学 | A kind of inorganic anti-corrosion pigment with molybdic acid zinc modification |
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| CN101428857B (en) | 2010-08-18 |
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