CN106744687B - A method of titanium hydride powders are prepared using chemical method - Google Patents
A method of titanium hydride powders are prepared using chemical method Download PDFInfo
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- CN106744687B CN106744687B CN201611106661.8A CN201611106661A CN106744687B CN 106744687 B CN106744687 B CN 106744687B CN 201611106661 A CN201611106661 A CN 201611106661A CN 106744687 B CN106744687 B CN 106744687B
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- titanium hydride
- hydride powders
- chemical method
- powders
- baking oven
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/02—Hydrides of transition elements; Addition complexes thereof
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- 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
Abstract
The invention discloses a kind of methods for preparing titanium hydride powders using chemical method, belong to Preparation Technique of Powders field.This method comprises the concrete steps that：It uses titanium valve for raw material, a certain amount of zinc powder and certain density sulfuric acid solution is added, prepare titantium hydride powder under normal pressure, 120 DEG C -230 DEG C of lower temperature.The present invention uses chemical method to be successfully prepared titanium hydride powders for the first time.It does not need that hydrogen is added in closed container during the preparation process, has not only saved cost, but also reduce the pollution to environment；Simultaneously because synthesis temperature is low, atmospheric operation, industrialized mass production easy to accomplish, to be expected to push the development of hydrogen storage material.
Description
Technical field
The invention belongs to Preparation Technique of Powders fields, and in particular to preparation TiH2The method of powder, more specifically, this hair
It is bright to be related to such a preparation TiH2The method of powder carries out hydrogenation treatment, using change using titanium valve as raw material in autoclave
Method prepares titanium hydride powders.
Background technique
Titantium hydride (TiH2) powder tool have been widely used.Can be used as metal and it is nonmetallic between bridging agent, more
Important purposes is as hydrogen storage material.Currently, the preparation of titantium hydride mainly uses titanium metal powder directly to add hydrogen at high temperature
Reaction obtains, expensive since the difficulty that these metal powders itself obtain is larger, with existing production method preparing hydrogen
Changing titanium, energy consumption is high, higher cost, is not suitable for the production of industrial mass, therefore limit the application of titantium hydride.Middle promulgated by the State Council
Bright patent CN200810300862.0 (publication date：On September 3rd, 2008) a kind of preparation method of titantium hydride is disclosed, it is by titanium
Raw material mixes under conditions of containing calcium or lithium with magnesium metal, is placed in closed container and is passed through hydrogen heating progress hydrogenation,
So that the titanium in reaction mass is transformed into titantium hydride, then will react gains acid and dissolve other impurity other than titantium hydride
Washout obtains titantium hydride；Chinese invention patent CN200780033193.9 (publication date：On September 5th, 2009) disclose a kind of incite somebody to action
Titanium valve material in process is used as raw material to prepare titantium hydride.It mainly include following key step：Titaniferous waste material is filled with
In reaction vessel；It removes the air in the reaction vessel and supplies hydrogen to the reaction vessel；And execute ball milling.More than
Patented method be directed to and be passed through hydrogen heating in closed container and carry out hydrogenation, and prepare the powder material of titantium hydride
Material.Undoubtedly, the cost for increasing reaction is not suitable for industrialized batch production.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method for preparing titanium hydride powders using chemical method,
To reduce preparation cost, reduces environmental pollution, push the development of hydrogen storage material.
A kind of method for preparing titanium hydride powders using chemical method of the present invention, this approach includes the following steps：
(1) it after mixing titanium valve, zinc powder with certain density sulfuric acid solution, is put into reaction vessel and seals；
The concentration of the sulfuric acid solution is 0.5~3mol/L, and the molar ratio of titanium valve and zinc powder is 1：10~80, the zinc powder
Molar ratio with sulfuric acid is 2~4：1；
(2) reaction vessel that step (1) seals is placed in 120~230 DEG C of baking oven, heats 2~6h；
(3) baking oven power supply is closed, by reaction vessel with baking oven cooled to room temperature, is washed, drying obtains hydride powder
End.
Further, the washing of the step (3) refers to：The centrifugation for being 2000~8000 revs/min in revolving speed by solution
Machine centrifugation, obtains sediment, sediment is re-dispersed into deionized water, filters, repeats the above steps, until the pH of filtrate
Value reaches 7.
Further, the reaction vessel is organic matter container or precious metal vessel.
Further, the reaction vessel is polytetrafluoroethylcontainer container.
The principles of science of the invention：Hydrogen is generated by zinc powder and sulfuric acid reaction, hydrogen occurs with titanium valve in closed environment
Change reaction, generates titantium hydride powder.
Compared with prior art, the present invention has the following technical effects：
1, it realizes for the first time and titantium hydride (TiH is prepared using chemical method2) powder.
2, what is be related to prepares titantium hydride synthesis method using chemical method, using titanium valve as raw material, and a certain concentration is added
Zinc powder and sulfuric acid solution, under the pressure that system itself generates, synthesizing hydrogenated titanium valve body under 120-230 DEG C of lower temperature.
This method low, atmospheric operation, industrialized mass production easy to accomplish because of synthesis temperature.
3, since the method that use is not passed through hydrogen in closed container prepares titantium hydride powder, cost has both been saved,
Reduce the pollution to environment again.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture for the titantium hydride powder that the embodiment of the present invention 1 obtains；
It was found from transmission electron microscope picture：Prepared TiH2The size of powder is about 80-100nm.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
1. ingredient：
(1) titanium valve for weighing 5mmol, which is added solvent and is 100 milliliters, use distilled water washed polytetrafluoroethylene (PTFE) appearance
In device.
(2) sulfuric acid solution for measuring 100ml 0.5mol/L is added in the mixture in above-mentioned polytetrafluoroethylcontainer container.
(3) 5.6g zinc powder is weighed to be added in above-mentioned solution.
(4) polytetrafluoroethylcontainer container is sealed, to guarantee reaction process cleaning.
2. heating：Baking oven is heated to 160 DEG C, the polytetrafluoroethylcontainer container of sealing is put into baking oven, reactant is made to exist
It is reacted 12 hours under above-mentioned condition, until reaction carries out completely.
3. cooling：After reaction reaches the scheduled time, baking oven power supply is closed, reaction vessel is gone with baking oven is naturally cold to room
Temperature.
4. washing：Solution is centrifuged in the centrifuge that revolving speed is 6000 revs/min, obtains sediment, again by sediment
It is distributed in deionized water, filters, repeat the above steps 6 times, until the pH value of filtrate reaches 7.
5. drying dries the powder being obtained by filtration at 80-100 DEG C or so, TiH is obtained2Nanometer powder.Transmitted electron is aobvious
Microcosmic examine shows that the size of powder is 80-100 nanometers of titantium hydride powder (see Fig. 1).
Embodiment 2
1. ingredient：
(1) titanium valve for weighing 5mmol, which is added solvent and is 100 milliliters, use distilled water washed polytetrafluoroethylene (PTFE) appearance
In device.
(2) sulfuric acid solution for measuring 100ml 1mol/L is added in the mixture in above-mentioned polytetrafluoroethylcontainer container.
(3) 22.4g zinc powder is weighed to be added in above-mentioned solution.
(4) polytetrafluoroethylcontainer container is sealed, to guarantee reaction process cleaning.
2. heating：Baking oven is heated to 200 DEG C, the polytetrafluoroethylcontainer container of sealing is put into baking oven, reactant is made to exist
It is reacted 24 hours under above-mentioned condition, until reaction carries out completely.
3. cooling：After reaction reaches the scheduled time, baking oven power supply is closed, reaction vessel is gone with baking oven is naturally cold to room
Temperature.
4. washing：Solution is centrifuged in the centrifuge that revolving speed is 6000 revs/min, obtains sediment, again by sediment
It is distributed in deionized water, filters, repeat the above steps 6 times, until the pH value of filtrate reaches 7.
5. drying dries the powder being obtained by filtration at 80-100 DEG C or so, TiH is obtained2Nanometer powder.Scanning electron is aobvious
Microcosmic examine shows that the size of powder is 100-120 nanometers of titantium hydride.
Embodiment 3
1. ingredient：
(1) titanium valve for weighing 10mmol, which is added solvent and is 100 milliliters, has used the washed polytetrafluoroethylene (PTFE) of distilled water
In container.
(2) sulfuric acid solution for measuring 100ml 2mol/L is added in the mixture in above-mentioned polytetrafluoroethylcontainer container.
(3) 33.6g zinc powder is weighed to be added in above-mentioned solution.
(4) polytetrafluoroethylcontainer container is sealed, to guarantee reaction process cleaning.
2. heating：Baking oven is heated to 230 DEG C, the polytetrafluoroethylcontainer container of sealing is put into baking oven, reactant is made to exist
It is reacted 36 hours under above-mentioned condition, until reaction carries out completely.
3. cooling：After reaction reaches the scheduled time, baking oven power supply is closed, reaction vessel is gone with baking oven is naturally cold to room
Temperature.
4. washing：Solution is centrifuged in the centrifuge that revolving speed is 6000 revs/min, obtains sediment, again by sediment
It is distributed in deionized water, filters, repeat the above steps 6 times, until the pH value of filtrate reaches 7.
5. drying：The powder being obtained by filtration is dried at 80-100 DEG C or so, obtains TiH2Nanometer powder.Scanning electron is aobvious
Microcosmic examine shows that the size of powder is 40-50 nanometers of titantium hydride.
Claims (4)
1. a kind of method for preparing titanium hydride powders using chemical method, this approach includes the following steps：
(1) it after mixing titanium valve, zinc powder with certain density sulfuric acid solution, is put into reaction vessel and seals；
The concentration of the sulfuric acid solution is 0.5~3mol/L, and the molar ratio of titanium valve and zinc powder is 1：10~80, the zinc powder and sulphur
The molar ratio of acid is 2~4：1；
(2) reaction vessel that step (1) seals is placed in 120~230 DEG C of baking oven, heats 2~6h；
(3) baking oven power supply is closed, by reaction vessel with baking oven cooled to room temperature, is washed, drying obtains titanium hydride powders；
The size of the titanium hydride powders is 40~120 nanometers.
2. a kind of method for preparing titanium hydride powders using chemical method as described in claim 1, which is characterized in that the step
Suddenly the washing of (3) refers to：Solution is centrifuged in the centrifuge that revolving speed is 2000~8000 revs/min, sediment is obtained, will precipitate
Object is re-dispersed into deionized water, is filtered, is repeated the above steps, until the pH value of filtrate reaches 7.
3. a kind of method for preparing titanium hydride powders using chemical method as described in claim 1, which is characterized in that described anti-
Answering container is organic matter container or precious metal vessel.
4. a kind of method for preparing titanium hydride powders using chemical method as claimed in claim 3, which is characterized in that described anti-
Answering container is polytetrafluoroethylcontainer container.
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| CN108217596B (en) * | 2018-01-29 | 2021-03-30 | 吉林大学 | Method for preparing niobium hydride and tantalum hydride by using non-hydrogen source solution method |
| CN113479844B (en) * | 2021-06-04 | 2022-11-01 | 中国原子能科学研究院 | Method for preparing titanium hydride by converting tritiated water sample |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254897A (en) * | 2008-04-08 | 2008-09-03 | 李健民 | Method for preparing titanium hydride |
| CN101511735A (en) * | 2006-09-07 | 2009-08-19 | 韩国生产技术研究院 | Manufacturing method for titanium hydride powders |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101511735A (en) * | 2006-09-07 | 2009-08-19 | 韩国生产技术研究院 | Manufacturing method for titanium hydride powders |
| CN101254897A (en) * | 2008-04-08 | 2008-09-03 | 李健民 | Method for preparing titanium hydride |
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