CN104418382B - A kind of hydrothermal method prepares the method for zinc metastannate - Google Patents

A kind of hydrothermal method prepares the method for zinc metastannate Download PDF

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Publication number
CN104418382B
CN104418382B CN201310407573.1A CN201310407573A CN104418382B CN 104418382 B CN104418382 B CN 104418382B CN 201310407573 A CN201310407573 A CN 201310407573A CN 104418382 B CN104418382 B CN 104418382B
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zinc
sodium hydroxide
solution
prepares
metastannate
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CN104418382A (en
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梁砚琴
崔振铎
杨贤金
朱胜利
郑静
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/38—Particle morphology extending in three dimensions cube-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a kind of method that hydrothermal method prepares zinc metastannate, adopt the method for Surfactant CTAB assisted hydrothermal synthesis, Zinc Sulphate Heptahydrate and cetyl trimethylammonium bromide are dissolved, again Tin tetrachloride pentahydrate and sodium hydroxide are dissolved, then constant temperature titration is carried out, and cool to room temperature with the furnace react 6h at 150 DEG C after, by the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, remove the foreign ion in precipitation, finally dry under 70 DEG C of air atmospheres and obtain final product.The present invention, by the consumption of regulation and control sodium hydroxide, prepares the different morphologies ZnSnO of size uniform, better crystallinity degree 3crystal.This kind of preparation method, easy to operate, with low cost, expense is low, consuming time short, is a kind of preparation method of efficient economy.

Description

A kind of hydrothermal method prepares the method for zinc metastannate
Technical field
The invention belongs to technical field of material, more particularly, relate to ZnSnO 3the preparation method of powder, is mainly used in gas sensitive field tests.
Background technology
Along with the raising of science and technology, people are also increasing for the demand of special material.But present stage material performance can not meet people produce and life needs.Along with going deep into of nanometer-micron technical, people are for the structure updating material, and the performance promoting material has had more deep understanding.Therefore research and develop functional material and have huge development space, meaning is also very great.
Hydrothermal synthesis method is a kind of important wet chemical method, and it can prepare the ZnSnO of different morphologies very easily 3nano/micron structure, causes extensive concern and the interest of the multi-disciplinary research personnel comprising materialogy thus.ZnSnO 3as a kind of sensitive material, people are to its applied research and propose high performance research further and also never interrupted.At present, hydrothermal method is adopted to prepare the ZnSnO of varied pattern 3nano/micron complex construction, more representational as 0 dimension (nanoparticle), 1 dimension (nano wire, nanometer rod), 3 dimensions (Nano microsphere, nano square, nanocage, polyhedron crystallite) etc.ZnSnO 3be a kind of important gas sensitive, have a wide range of applications.It is to CO, H 2s, i-butane, CH 4, LPG, CH 3sH, NO xdeng there being gas sensing property.ZnSnO 3easily Zn is transformed into more than 700 DEG C 2snO 4and SnO 2.And Zn 2snO 4air-sensitive performance poor, be the product not wishing to obtain.Therefore the preparation method of material has very large impact to the sensitivity of gas and response-turnaround time etc.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of simple and convenient, the with low cost hydrothermal method that utilizes prepares ZnSnO 3method.
Technical scheme of the present invention is achieved by following technical proposals:
A kind of hydrothermal method prepares ZnSnO 3method, carry out according to following step:
Step 1, by Zinc Sulphate Heptahydrate (ZnSO 47H 2and cetyl trimethylammonium bromide (C O) 16h 33(CH 3) 3nBr, CTAB) be dissolved in 20mL distilled water, form the first solution;
Step 2, by Tin tetrachloride pentahydrate (SnCl 45H 2o) and sodium hydroxide (NaOH) dissolve in 20mL distilled water, form the second solution;
Step 3, first solution is placed in 60 DEG C of water bath with thermostatic control magnetic stirring apparatuss, after homo(io)thermism, second solution instills in the first solution again, after keeping magnetic agitation 30-60min, suspension liquid is proceeded in reactor, after reacting 6h at being then placed in 150 DEG C, cool to room temperature (namely 20-25 DEG C) with the furnace;
Step 4, by the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains final product.
In technique scheme, the mass ratio of each medicine is ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:11, obtains the ZnSnO of simple cubic structure 3, size, between 40-80nm, is evenly distributed.
In technique scheme, the mass ratio of each medicine is ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:20, obtains the ZnSnO of lamellar structure 3, size, between 100-200nm, is evenly distributed.
In technique scheme, the mass ratio of each medicine is ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:60, obtains the ZnSnO of 14 body structures 3, size, between 150-250nm, is evenly distributed.
In technique scheme, in step 3, magnetic agitation selects 150-200 turns/min, and rate of addition is 0.1-0.5ml/min.
The present invention adopts the method for Surfactant CTAB assisted hydrothermal synthesis, dense by regulation and control soda acid, prepares the ZnSnO of different morphologies of size uniform, better crystallinity degree 3crystal.Based on the ABO that this kind of method is prepared 3the ZnSnO of structure 3nano material, by investigating the impact of change on Product size and pattern of synthesis condition, discloses the formation mechenism of this kind of crystal.This kind of preparation method, easy to operate, with low cost, expense is low, consuming time short, is a kind of preparation method of efficient economy.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the embodiment of the present invention 1 preparing product.
Fig. 2 is the stereoscan photograph of the embodiment of the present invention 2 preparing product.
Fig. 3 is the stereoscan photograph of the embodiment of the present invention 3 preparing product.
Fig. 4 is the XRD test curve of embodiment product prepared by the present invention, and wherein a is embodiment 1, b be embodiment 2, c is embodiment 3.
Embodiment:
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1:
The mass ratio of each medicine is: ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:11.
Take the ZnSO of 0.259g 47H 2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g 45H 2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.23gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 150 turns/min, and rate of addition is 0.5ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension liquid is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of loft drier react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains final product, and as shown in Figure 1, the structure shown in accompanying drawing 1 is the ZnSnO of simple cubic structure 3, size, between 40-80nm, is evenly distributed.
Embodiment 2:
The mass ratio of each medicine is: ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:20.
Take the ZnSO of 0.259g 47H 2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g 45H 2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.4gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 200 turns/min, and rate of addition is 0.1ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension liquid is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of loft drier react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains final product, and as shown in Figure 2, the structure shown in accompanying drawing 2 is the ZnSnO of lamellar structure 3, size, between 100-200nm, is evenly distributed.
Embodiment 3:
The mass ratio of each medicine is: ZnSO 47H 2o:SnCl 45H 2o:CTAB:NaOH is 13:16:5:60.
Take the ZnSO of 0.259g 47H 2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g 45H 2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.6gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 180 turns/min, and rate of addition is 0.3ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension liquid is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of loft drier react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains final product, and as shown in Figure 3, the structure shown in accompanying drawing 3 is the ZnSnO of 14 body structures 3, size, between 150-250nm, is evenly distributed.
Product prepared by embodiment 1-3 is carried out XRD test, and result is by shown in accompanying drawing 4, although the pattern of product is shown as three kinds of different patterns, the final product of three kinds of preparation methods is ZnSnO 3.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.

Claims (2)

1. hydrothermal method prepares a method for zinc metastannate, it is characterized in that, carries out according to following step:
Step 1, is dissolved in Zinc Sulphate Heptahydrate and cetyl trimethylammonium bromide in 20mL distilled water, forms the first solution;
Step 2, dissolves Tin tetrachloride pentahydrate and sodium hydroxide in 20mL distilled water, forms the second solution;
Step 3, is placed in 60 DEG C of water bath with thermostatic control magnetic stirring apparatuss, after homo(io)thermism by the first solution, again the second solution is instilled in the first solution, after keeping magnetic agitation 30-60min, suspension liquid is proceeded in reactor, after reacting 6h at being then placed in 150 DEG C, cool to room temperature with the furnace;
Step 4, by the white precipitate deionized water collected and dehydrated alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains final product;
Wherein the mass ratio of each medicine is Zinc Sulphate Heptahydrate: Tin tetrachloride pentahydrate: cetyl trimethylammonium bromide: sodium hydroxide is 13:16:5:11, and obtain the zinc metastannate of simple cubic structure, size, between 40-80nm, is evenly distributed; The mass ratio of each medicine is Zinc Sulphate Heptahydrate: Tin tetrachloride pentahydrate: cetyl trimethylammonium bromide: sodium hydroxide is 13:16:5:20, and obtain the zinc metastannate of lamellar structure, size, between 100-200nm, is evenly distributed; The mass ratio of each medicine is Zinc Sulphate Heptahydrate: Tin tetrachloride pentahydrate: cetyl trimethylammonium bromide: sodium hydroxide is 13:16:5:60, and obtain the zinc metastannate of 14 body structures, size, between 150-250nm, is evenly distributed.
2. a kind of hydrothermal method according to claim 1 prepares the method for zinc metastannate, it is characterized in that, in step 3, magnetic agitation selects 150-200 turns/min, and rate of addition is 0.1-0.5mL/min.
CN201310407573.1A 2013-09-09 2013-09-09 A kind of hydrothermal method prepares the method for zinc metastannate Expired - Fee Related CN104418382B (en)

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CN105405656B (en) * 2015-11-30 2018-07-20 福州大学 A kind of graded structure Zn2SnO4And its application
CN105776322A (en) * 2016-05-24 2016-07-20 江苏大学 Porous zinc metastannate hollow sphere material and preparation method thereof
CN109187662A (en) * 2018-08-31 2019-01-11 天津大学 Work in the metal oxide base ethyl alcohol gas sensor preparation method of room temperature
CN109179488A (en) * 2018-08-31 2019-01-11 天津大学 A kind of preparation method of 3D cube frame structure ternary metal oxide semiconductor zinc metastannate
CN110180526B (en) * 2019-05-10 2022-03-25 重庆第二师范学院 Photocatalyst Li2SnO3The preparation method and the application thereof in degrading antibiotics
CN110108758B (en) * 2019-05-13 2022-05-24 上海理工大学 Formaldehyde sensitive material, sensitive element and preparation method thereof
CN111348677B (en) * 2020-03-10 2022-06-10 景德镇学院 Preparation method and application of zinc metastannate nanofiber gas-sensitive material

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