CN103864032B - A kind of preparation method of nano material - Google Patents
A kind of preparation method of nano material Download PDFInfo
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- CN103864032B CN103864032B CN201410121032.7A CN201410121032A CN103864032B CN 103864032 B CN103864032 B CN 103864032B CN 201410121032 A CN201410121032 A CN 201410121032A CN 103864032 B CN103864032 B CN 103864032B
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Abstract
The present invention relates to a kind of preparation method of titanium nitride nano material, belong to technical field of inorganic nanometer material.First with natural fiber element material for template, take tetrabutyl titanate as titanium precursor, prepare the titania nanotube to cellulosic material with similar microscopic appearance and hierarchical structure, then use MAGNESIUM METAL to make reductive agent, in high temperature (1100 DEG C-1300 DEG C) tube furnace, prepare the TiN nano material with three-dimensional communication pore passage structure by the method for magnesiothermic reduction.The TiN nano material utilizing the present invention to prepare has complicated three-dimensional communication pore passage structure, the uniform tube wall of thickness, higher specific surface area and pore volume, and therefore this TiN nano material with complicated three-dimensional communication pore passage structure is expected to there is good application prospect in catalysis and fractionation by adsorption field.
Description
The present patent application is application number 201210241535.9, the applying date on 07 12nd, 2012, the divisional application of denomination of invention " a kind of titanium nitride nano material and preparation method with three-dimensional communication pore passage structure ".
Technical field
The present invention relates to a kind of preparation method of nano material, be specifically related to a kind of preparation method of titanium nitride nano material.
Background technology
Titanium nitride (TiN) is a kind of transition metal nitride, there is B1 – NaCl type crystal structure, because of the physics and chemistry character of its excellence, such as high rigidity, high-melting-point, excellent specific conductivity, thermal conductivity and erosion resistance, and high chemical stability, there is important using value in engineer applied, therefore receive the very big concern of investigator.But little about the research of three-dimensional nitride nano-material, the unicity of resulting materials microtexture and pattern limits it in application that is industrial and field of engineering technology.Therefore, the novel TiN nano material with three-dimensional structure and complex topography is researched and developed imperative with the active demand meeting actual production and life.
As the natural fiber element material of the important a member of biological template, the abundantest in distributed in nature, there is unique and complex three-dimensional hierarchical structure, application natural fiber element material is that template and skeleton preparation have the functional materials of multilayered structure and pattern, is one and prepares easy, the low cost of functional materials and the synthesis shortcut of environmental protection.Magnesium reduction process utilizes the compound of the active more weak metal of magnesium metal reduction to produce the process of metal simple-substance or its alloy, and reaction process is simple, and intermediate product magnesium oxide only can need be removed by simple acid treatment.Chinese invention patent CN 101357762A, CN 101348242A and CN 102259858 describes the method using magnesium reduction process to prepare zirconium carbide powder, boron nitride nano-tube and porous elemental silicon respectively in detail.At present, magnesium reduction process has very consequence in field of material preparation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with the nano material of three-dimensional communication pore passage structure.
The inventive method specifically comprises the following steps, a kind of preparation method with the titanium nitride nano material of three-dimensional communication pore passage structure:
(1) join in organic solvent by the concentrated hydrochloric acid of 36% and tetrabutyl titanate successively under whipped state, Keep agitation 3 h obtains TiO 2 sol.Wherein, tetrabutyl titanate followed by raw material: dense HCl: the mass ratio of organic solvent=7:5:50 ~ 100;
(2) natural fiber prime modulus plate is dipped in above-mentioned solution, leaves standstill after 3 ~ 12 h and take out, deionized water wash number all over after put into 40 ~ 65 ° of C loft drier dried overnight; Dried sample is raised to 450 ~ 600 ° of C roasting 4 ~ 6 h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material;
(3) under room temperature, in nitrogen atmosphere by above gained titania nanotube and MAGNESIUM METAL particle be placed in two ends, left and right in homemade stainless steel cauldron respectively according to the mol ratio of 1:2.5 ~ 4, do not contact each other; Inflated with nitrogen in reactor is put into tube furnace be rapidly heated (temperature rise rate 10 ° of C/min) to 1100 ~ 1300 DEG C of maintenance 2 ~ 5 h, rear cool to room temperature except seal after net air;
(4) reaction product 1 ~ 2 M dilute acid solution process 6 ~ 10 h is removed by product MgO, obtain target product.
In the present invention, organic solvent described in step (1) is dehydrated alcohol or dehydrated alcohol/toluene (volume ratio 1:1) mixed solution.
In the present invention, natural fiber prime modulus plate described in step (2) is the one in quantitative paper, hospital gauze, absorbent cotton.
In the present invention, described in step (4), diluted acid is dilute hydrochloric acid or dust technology.
The present invention has following beneficial effect:
The titanium nitride nano material that the present invention prepares has more advantage than one dimension titanium nitride material in mass transfer.Target product has larger specific surface area and pore volume, and traditional solid nitride powder Particle Phase ratio, has more wide application prospect in catalysis and fractionation by adsorption field.Use filter paper, absorbent cotton or gauze for stay in place form in preparation process, by selecting suitable preparation condition, macroscopically be there is the titanium nitride nano material of scraps of paper shape, cotton-wool dress and gauze shape, these materials with macro morphology directly can be brought application, save conventional preparation techniques product mostly be powder, need the step of further compression moulding before using.
Accompanying drawing explanation
Fig. 1 be preparation have three-dimensional communication pore passage structure titanium nitride nano material SEM figure.
Fig. 2 be preparation have three-dimensional communication pore passage structure the XRD figure of titanium nitride nano material.
Embodiment
Below by embodiment, the present invention is further described.
Embodiment 1
(1) join in dehydrated alcohol by the concentrated hydrochloric acid of 36% and tetrabutyl titanate successively under whipped state, Keep agitation 3 h obtains TiO 2 sol.Wherein, tetrabutyl titanate: dense HCl: the mass ratio of dehydrated alcohol=7:5:100;
(2) common for use for laboratory quantitative paper is dipped in above-mentioned solution, takes out after leaving standstill 3 h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material;
(3), under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are above placed in two ends, left and right in homemade stainless steel cauldron respectively according to the mol ratio of 1:2.5, do not contact each other; Sealed after inflated with nitrogen in reactor 2 h Ex-all wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1200 DEG C keep 2 h, after be cooled to room temperature;
(4) reaction product 2 M diluted hydrochloric acid aqueous solution process 6 h are removed by product MgO, obtain target product.
Embodiment 2
(1) successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol/toluene mixture (volume ratio 1:1) under whipped state, Keep agitation 3 h.Wherein, tetrabutyl titanate followed by raw material: dense HCl: the mass ratio of dehydrated alcohol/toluene=7:5:100;
(2) medical gauze is dipped in above-mentioned solution, takes out after leaving standstill 3 h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material;
(3), under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are placed in two ends, left and right in homemade stainless steel cauldron respectively according to the mol ratio of 1:4, do not contact each other; Sealed after inflated with nitrogen in reactor 2 h Ex-all wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1100 DEG C keep 2 h, after be cooled to room temperature;
(4) reaction product 2 M diluted hydrochloric acid aqueous solution process 6 h are removed by product MgO, obtain target product.
Embodiment 3
(1) successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol under whipped state, Keep agitation 3 h.Wherein, tetrabutyl titanate: dense HCl: the mass ratio of dehydrated alcohol=7:5:50;
(2) common for use for laboratory quantitative paper is dipped in above-mentioned solution, takes out after leaving standstill 3 h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material;
(3), under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are above placed in two ends, left and right in homemade stainless steel cauldron respectively according to the mol ratio of 1:2.5, do not contact each other; Sealed after inflated with nitrogen in reactor 2 h Ex-all wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1300 DEG C keep 2 h, after be cooled to room temperature;
(4) reaction product 1 M diluted nitric acid aqueous solution process 10 h is removed by product MgO, obtain target product.
Claims (1)
1. a preparation method for titanium nitride nano material, is characterized in that, according to the following steps:
(1) join in dehydrated alcohol by the concentrated hydrochloric acid of 36% and tetrabutyl titanate successively under whipped state, Keep agitation 3 h obtains TiO 2 sol; Wherein, tetrabutyl titanate: dense HCl: the mass ratio of dehydrated alcohol=7:5:100;
(2) common for use for laboratory quantitative paper is dipped in above-mentioned solution, takes out after leaving standstill 3 h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material;
(3), under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are above placed in two ends, left and right in stainless steel cauldron respectively according to the mol ratio of 1:2.5, do not contact each other; Sealed after inflated with nitrogen in reactor 2 h Ex-all wherein air, put into tube furnace and be rapidly heated to about 1200 DEG C with the temperature rise rate of 10 ° of C/min and keep 2 h, after be cooled to room temperature;
(4) reaction product 2 M diluted hydrochloric acid aqueous solution process 6 h are removed by product MgO, obtain target product.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210241535.9A CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
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| CN201210241535.9A Division CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
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| CN103864032A CN103864032A (en) | 2014-06-18 |
| CN103864032B true CN103864032B (en) | 2015-09-23 |
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| CN201210241535.9A Expired - Fee Related CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
| CN201410121084.4A Expired - Fee Related CN103864033B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of titanium nitride material |
| CN201410120722.0A Expired - Fee Related CN103864031B (en) | 2012-07-12 | 2012-07-12 | Method for preparing nano-material with high specific surface area and pore volume |
| CN201410121032.7A Expired - Fee Related CN103864032B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of nano material |
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| CN201410121084.4A Expired - Fee Related CN103864033B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of titanium nitride material |
| CN201410120722.0A Expired - Fee Related CN103864031B (en) | 2012-07-12 | 2012-07-12 | Method for preparing nano-material with high specific surface area and pore volume |
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| CN103450475B (en) * | 2013-09-13 | 2015-10-21 | 中北大学 | The preparation method of core-shell structural conductive polyaniline/Co3O4 powder |
| CN103736475B (en) * | 2014-01-08 | 2015-08-19 | 国家纳米科学中心 | A kind of three-dimensional porous titanium dioxide nano tube catalyst, preparation method and its usage |
| CN105502316B (en) * | 2016-01-30 | 2018-01-12 | 武汉科技大学 | A kind of nitride powder based on low temperature liquid polymerization process and preparation method thereof |
| CN107675483B (en) * | 2017-09-21 | 2019-08-06 | 东华大学 | A kind of preparation method of the titania nanotube based on click chemistry/cotton fabric catalysis material |
| CN108213461B (en) * | 2017-12-12 | 2021-07-16 | 昆明理工大学 | Preparation method of nano-grade noble metal material |
| CN108298957A (en) * | 2018-02-06 | 2018-07-20 | 叶剑 | A kind of preparation method of 3 D stereo nano material |
| CN110606487A (en) * | 2019-10-16 | 2019-12-24 | 大连理工大学 | Honeycomb three-dimensional porous MXene with controllable pore diameter and general synthesis method thereof |
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| CN101811677B (en) * | 2010-05-06 | 2011-11-09 | 东华大学 | Method for preparing hollow porous quadruped titanium nitride |
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| Publication number | Publication date |
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| CN103864031B (en) | 2015-07-22 |
| CN103864031A (en) | 2014-06-18 |
| CN102701163A (en) | 2012-10-03 |
| CN103864032A (en) | 2014-06-18 |
| CN103864033A (en) | 2014-06-18 |
| CN102701163B (en) | 2014-03-19 |
| CN103864033B (en) | 2016-01-20 |
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