CN103864033B - A kind of preparation method of titanium nitride material - Google Patents
A kind of preparation method of titanium nitride material Download PDFInfo
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- CN103864033B CN103864033B CN201410121084.4A CN201410121084A CN103864033B CN 103864033 B CN103864033 B CN 103864033B CN 201410121084 A CN201410121084 A CN 201410121084A CN 103864033 B CN103864033 B CN 103864033B
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Abstract
The present invention relates to a kind of preparation method with the titanium nitride nano material of three-dimensional communication pore passage structure, 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 invention belongs to technical field of 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.In recent years, research about nanostructure TiN has more research, but existing report is mainly around preparation and the character research of titanium nitride nano particle and titanium nitride membrane, research about three-dimensional nitride nano-material is little, and the unicity of resulting materials microtexture and pattern limits it in application that is industrial and field of engineering technology.Biological template nano materials refers to have the biological tissue of suitable construction for template, utilizes self-assembly and space confinement effect, forms the nano material of given structure or the process of nanostructure by the method such as physics, chemistry.The structural unit of many biological tissues is all in nanometer range, and these biological structure unit with nanoscale or nano aperture all can be used as template to prepare nano material.Due to the various advantages (size of Nano grade, diversified profile, nature rich content and environmental friendliness etc.) of biomolecules, take biological tissue as template, the artificial material nano material by self assembly with complicated nanostructure and microscopic appearance is an extremely potential research direction.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.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with the titanium nitride nano material of three-dimensional communication pore passage structure.
Method provided by the invention, 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 3h obtains TiO 2 sol.Wherein, tetrabutyl titanate followed by raw material: dense HCl: the mass ratio of organic solvent=7:5:50 ~ 100; Described organic solvent is dehydrated alcohol or dehydrated alcohol/toluene (volume ratio 1:1) mixed solution.
(2) natural fiber prime modulus plate is dipped in above-mentioned solution, leaves standstill after 3 ~ 12h 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 ~ 6h removing templates with the temperature rise rate of 2 ° of C/min and obtains titania nanotube material; Described natural fiber prime modulus plate is the one in quantitative paper, hospital gauze, absorbent cotton.
(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 ~ 5h, rear cool to room temperature except seal after net air;
(4) reaction product 1 ~ 2M dilute acid solution process, 6 ~ 10h is removed by product MgO, obtain target product.Described diluted acid is dilute hydrochloric acid or dust technology.
The present invention has following beneficial effect:
The titanium nitride material that the present invention prepares is the nano pore structure with three-dimensional communication, in mass transfer, have advantage.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.
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) successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol/toluene mixture (volume ratio 1:1) under whipped state, Keep agitation 3h.Wherein, tetrabutyl titanate followed by raw material: dense HCl: the mass ratio of dehydrated alcohol/toluene=7:5:100;
(2) absorbent cotton is dipped in above-mentioned solution, takes out after leaving standstill 3h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5h 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 2h Ex-all in reactor wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1300 DEG C keep 2h, after be cooled to room temperature;
(4) reaction product 2M diluted hydrochloric acid aqueous solution process 6h is 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 3h.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 3h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5h 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 2h Ex-all in reactor wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1100 DEG C keep 2h, after be cooled to room temperature;
(4) reaction product 2M diluted hydrochloric acid aqueous solution process 6h is 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 3h.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 3h, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5h 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 2h Ex-all in reactor wherein air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1300 DEG C keep 2h, after be cooled to room temperature;
(4) reaction product 1M diluted nitric acid aqueous solution process 10h is removed by product MgO, obtain target product.
Claims (1)
1. a preparation method for titanium nitride material, is characterized in that, according to the following steps:
(1) successively the concentrated hydrochloric acid of 36% and tetrabutyl titanate being joined volume ratio under whipped state is that in the dehydrated alcohol/toluene mixture of 1:1, Keep agitation 3h obtains TiO 2 sol; Wherein, tetrabutyl titanate: dense HCl: the mass ratio of dehydrated alcohol/toluene=7:5:50;
(2) absorbent cotton is dipped in above-mentioned solution, takes out after leaving standstill 12h, by deionized water wash number time, put into 40 DEG C of loft drier dried overnight; Dried sample is raised to 600 DEG C of roasting 6h removing templates with the temperature rise rate of 2 DEG 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 1:4, do not contact each other; Sealed after inflated with nitrogen 2h Ex-all in reactor wherein air, put into tube furnace with the temperature rise rate of 10 DEG C/min be rapidly heated to 1100 DEG C keep 5h, after be cooled to room temperature;
(4) reaction product 1M diluted nitric acid aqueous solution process 10h is 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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| CN103864033A CN103864033A (en) | 2014-06-18 |
| CN103864033B true CN103864033B (en) | 2016-01-20 |
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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 |
| CN201410121032.7A Expired - Fee Related CN103864032B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of nano 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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| CN201410121032.7A Expired - Fee Related CN103864032B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of nano 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101811677A (en) * | 2010-05-06 | 2010-08-25 | 东华大学 | Method for preparing hollow porous quadruped titanium nitride |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811677A (en) * | 2010-05-06 | 2010-08-25 | 东华大学 | Method for preparing hollow porous quadruped titanium nitride |
Non-Patent Citations (2)
| Title |
|---|
| "Tubular structured hierarchical mesoporous titania material derived from natural cellulosic substances and application as photocatalyst for degradation of methylene blue";Haiqing Huang等;《Materials Research Bulletin》;20110805(第46期);摘要以及第1815页左栏第4段 * |
| "天然纤维素为模板的氮化钛纳米管的制备";刘效艳等;《中国化学会第28届学术年会第4分会场摘要集》;20120413;第1-2段以及图1 * |
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| CN102701163B (en) | 2014-03-19 |
| CN103864031B (en) | 2015-07-22 |
| CN102701163A (en) | 2012-10-03 |
| CN103864033A (en) | 2014-06-18 |
| CN103864032B (en) | 2015-09-23 |
| CN103864032A (en) | 2014-06-18 |
| CN103864031A (en) | 2014-06-18 |
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