CN101306833B - Microwave method for preparing cadmium hydroxide nano materials - Google Patents
Microwave method for preparing cadmium hydroxide nano materials Download PDFInfo
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- CN101306833B CN101306833B CN2008100401571A CN200810040157A CN101306833B CN 101306833 B CN101306833 B CN 101306833B CN 2008100401571 A CN2008100401571 A CN 2008100401571A CN 200810040157 A CN200810040157 A CN 200810040157A CN 101306833 B CN101306833 B CN 101306833B
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Abstract
The invention relates to a method for preparing a cadmium hydride nano material by microwaves. In the method, cadmium salt is dissolved in water, the mixture is added with ammonia water or sodium hydroxide to form clear and transparent cadmium complex ion solution, the solution is added with water insoluble fatty alcohol, and a fatty alcohol-water interface system is taken as reaction medium, the microwave irradiation technique is adopted, the microwave power and the reaction time are controlled, surface active agents are added to change the size and the shape of products, and finally the cadmium hydride nano material is prepared. The method has the advantages of simple operation procedure, fast reaction and low cost, and cadmium hydride nano materials prepared by the method can be well applied in the fields such as the packaging and releasing of batteries and drugs and the catalyzing separation, etc.
Description
Technical field
The present invention relates to a kind of microwave preparation of cadmium hydroxide nano materials, being specifically related to a kind of is reaction medium with the interface system, adopts the microwave exposure technology to prepare the method for cadmium hydroxide nano materials.The invention belongs to the nano material preparation technical field.
Background technology
Nano material has received the very big concern of people because of its functions peculiar and character, it has important effect in various fields such as nanoelectronics, magnetics, photoelectronics, therefore the control of nano material is synthetic has been subjected to increasing attention, and the preparation method emerges in an endless stream.Wherein interfacial synthesis has characteristics such as spontaneous, quick, that motivating force is low, has been subjected to good application, and the differential responses thing is in separately the environment, helps the product nucleation, the morphology control during crystallization.In addition, nucleus is by the transfer in different solutions, and the replacement of surface adsorption agent changes its solubleness in different solutions, thereby can obtain orderly nanoparticle.If his householder method such as microwave exposure method in conjunction with other more can obtain beyond thought result.
Hollow nanostructures may has low density because of it, high surface area, and special advantages such as optical property have been subjected to widely and have paid close attention to, and in drug encapsulation, release, aspects such as catalytic separation have well to be used.The synthetic method of hollow nanostructures may mainly concentrates on template, and template is sacrificed method, sol-gel method, and tensio-active agent/superpolymer assistance method etc., these method complicated operations are unfavorable for the widespread use of material synthetic.By contrast, interfacial synthesis is simple to operate, controllable product shape, and have universality, be easy to realize the synthetic of different-shape nano material.
Cadmium hydroxide can increase the loading capacity of nickel/cadmium cell well as electrode additive, and can reduce the self-discharge of electrode itself.And because the application of cadmium hydroxide aspect separation anionic dyestuff and DNA in recent years, its preparation method receives publicity more.Wherein hydrothermal method is that (Chinese invention patent: the synthetic method of cadmium hydroxide monocrystal nanowire, publication number: CN1546382), but this method required time is longer, and its limitation is arranged for the method that is commonly used to prepare the nanostructure cadmium hydroxide.
Summary of the invention
The object of the invention is at the deficiencies in the prior art, and a kind of microwave preparation of cadmium hydroxide nano materials is provided, and technology is simple, and production cost is low, and the cadmium hydroxide nano materials of gained can further satisfy industrial requirement.
For realizing such purpose, in technical scheme of the present invention, earlier cadmium salt is dissolved in the water, adds ammoniacal liquor or sodium hydroxide, be mixed with the cadmium complexing ion solution of clear, add water-fast Fatty Alcohol(C12-C14 and C12-C18) then, with Fatty Alcohol(C12-C14 and C12-C18)-water termination system is reaction medium, adopts the microwave exposure technology, controlled microwave power and reaction times, and add size and the pattern that tensio-active agent changes product, can prepare cadmium hydroxide nano materials.
Method of the present invention is specially:
By weight, 1-10 part cadmium salt is dissolved in 1000 parts the water, the cadmium complexing ion solution that adds ammoniacal liquor or sodium hydroxide formation clear then, the Fatty Alcohol(C12-C14 and C12-C18) that adds 100-1000 part then, and add tensio-active agent 1-10 part, stir, left standstill 1-2 hour, then reaction solution is transferred in the tetrafluoroethylene reactor pulse microwave irradiation 1-10 minute, pulse microwave power 300w-800w; After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and promptly obtains cadmium hydroxide nano materials.
Cadmium salt described in the present invention is cadmium acetate, cadmium nitrate or Cadmium Sulphate.
Fatty Alcohol(C12-C14 and C12-C18) of the present invention is a propyl carbinol, n-hexyl alcohol, n-Octanol butyleneglycol or glycerol.
Tensio-active agent of the present invention is that sodium lauryl sulphate, cetyl trimethylammonium bromide or song draw ketone.
The inventive method is simple, and interface system is a reaction medium, be reaction template and guide effect be provided, and product in homophase not transfer and the replacement of surface adsorption agent, make nanoparticle have homogeneity preferably.Adopted the microwave exposure technology, can improve the crystallization velocity of product on the one hand, operation steps is simple on the other hand, and cost is low, and speed of response is fast, the efficient height, and have certain universality.
The cadmium hydroxide nano materials of the present invention's preparation can be in battery, drug encapsulation, release, and there is good application aspects such as catalytic separation.
Description of drawings
Fig. 1 is the cadmium hydroxide transmission electron microscope photo of the embodiment of the invention 1 gained.
Fig. 2 is the cadmium hydroxide transmission electron microscope photo of the embodiment of the invention 2 gained.
Fig. 3 is the cadmium hydroxide transmission electron microscope photo of the embodiment of the invention 3 gained.
Fig. 4 is the cadmium hydroxide transmission electron microscope photo of the embodiment of the invention 4 gained.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.Following embodiment further specifies of the present invention, and does not limit the scope of the invention.
Embodiment 1
1. in the reaction flask of a 30ml, 1 part of cadmium salt is dissolved in 1000 parts the water, add the cadmium complexing ion solution that strong aqua forms clear then, add 100 parts of n-Octanols then, 1 part of sodium lauryl sulphate, vigorous stirring left standstill 2 hours.
2. will transfer in the 50ml tetrafluoroethylene reactor pulse microwave irradiation 3 minutes, pulse microwave power 500w according to the reaction solution that 1. step prepares.After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and can obtain cadmium hydroxide nano materials.
Fig. 1 is the transmission electron microscope photo and the electron-diffraction diagram of the cadmium hydroxide nano materials that obtains.As seen from the figure, cadmium hydroxide nano materials is polycrystalline one dimension item chain structure, and is assembled by the secondary structure of hollow ball.
Embodiment 2
1. in the reaction flask of a 30ml, 10 parts of cadmium salts are dissolved in 1000 parts the water, add the cadmium complexing ion solution that 100 parts of sodium hydroxide form clears then, add 1000 parts of n-Octanols then, 1 part of song draws ketone, and vigorous stirring left standstill 1 hour.
2. will transfer in the 50ml tetrafluoroethylene reactor pulse microwave irradiation 10 minutes, pulse microwave power 300w according to the reaction solution that 1. step prepares.After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and can obtain cadmium hydroxide nano materials.
The transmission electron microscope photo of resulting cadmium hydroxide nano materials as shown in Figure 2.As seen from the figure, cadmium hydroxide nano materials is the hexagonal chip architecture.
Embodiment 3
1. in the reaction flask of a 30ml, 10 parts of cadmium salts are dissolved in 1000 parts the water, add the cadmium complexing ion solution that strong aqua forms clear then, add 1000 parts of n-Octanols, add 6 parts of sodium lauryl sulphate then, vigorous stirring 1 minute left standstill 2 hours.
2. will transfer in the 50ml tetrafluoroethylene reactor pulse microwave irradiation 1 minute, pulse microwave power 800w according to the reaction solution that 1. step prepares.After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and can obtain cadmium hydroxide hollow nano material.
The transmission electron microscope photo of resulting cadmium hydroxide nano materials as shown in Figure 3.As seen from the figure, cadmium hydroxide nano materials is short one dimension item chain structure, but is assembled by the secondary structure of hollow ball.
Embodiment 4
1. in the reaction flask of a 30ml, 10 parts of cadmium salts are dissolved in 1000 parts the water, add the cadmium complexing ion solution that strong aqua forms clear then, add 1000 parts of n-Octanols, and adding 10 parts of cetyl trimethylammonium bromides, vigorous stirring 1 minute left standstill 2 hours.
2. will transfer in the 50ml tetrafluoroethylene reactor pulse microwave irradiation 3 minutes, pulse microwave power 500w according to the reaction solution that 1. step prepares.After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and can obtain cadmium hydroxide nano materials.
The transmission electron microscope photo of resulting cadmium hydroxide nano materials as shown in Figure 4.As seen from the figure, cadmium hydroxide nano materials is hollow ball structure.
Claims (3)
1. the microwave preparation of a cadmium hydroxide nano materials, it is characterized in that: by weight, 1-10 part cadmium salt is dissolved in 1000 parts the water, adds the cadmium complexing ion solution that ammoniacal liquor forms clear then, the Fatty Alcohol(C12-C14 and C12-C18) that adds 100-1000 part then, and adding tensio-active agent 1-10 part, stir, left standstill 1-2 hour, reaction solution is transferred in the tetrafluoroethylene reactor then, pulse microwave irradiation 1-10 minute, pulse microwave power 300w-800w; After reaction finished, reactor naturally cooled to 60 ℃, and product is filtered, and with dehydrated alcohol, water washing for several times, vacuum is drained, and promptly obtains cadmium hydroxide nano materials; Described tensio-active agent is sodium lauryl sulphate or cetyl trimethylammonium bromide.
2. according to the microwave preparation of the cadmium hydroxide nano materials of claim 1, it is characterized in that described cadmium salt is cadmium acetate, cadmium nitrate or Cadmium Sulphate.
3. according to the microwave preparation of the cadmium hydroxide nano materials of claim 1, it is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) is a propyl carbinol, n-hexyl alcohol, n-Octanol, butyleneglycol or glycerol.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102432061A (en) * | 2011-09-29 | 2012-05-02 | 新疆大学 | Method for preparing Cd(OH)2 and CdO hexagonal nanoplates in simple solvent system |
| CN103073049A (en) * | 2011-10-26 | 2013-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Complexing-agent-assisted preparation method of cadmium sulfide multi-level-structured nano-grade material |
| CN106379930A (en) * | 2016-11-09 | 2017-02-08 | 上海天地涂料有限公司 | Interface microwave preparation method of zinc oxide nanometer material |
| CN112897573B (en) * | 2019-12-03 | 2022-03-18 | 中国科学院深圳先进技术研究院 | Cadmium hydroxide porous material, preparation method thereof, and cathode and battery comprising cadmium hydroxide porous material |
| CN112897572B (en) * | 2019-12-03 | 2022-05-27 | 中国科学院深圳先进技术研究院 | Two-dimensional cadmium hydroxide material, preparation method, growth template and application |
| CN114702059B (en) * | 2021-12-30 | 2023-06-06 | 南京大学 | Binary hydroxide nanotube with composite structure and preparation method thereof |
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