CN101254897A - Method for preparing titanium hydride - Google Patents
Method for preparing titanium hydride Download PDFInfo
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- CN101254897A CN101254897A CNA2008103008620A CN200810300862A CN101254897A CN 101254897 A CN101254897 A CN 101254897A CN A2008103008620 A CNA2008103008620 A CN A2008103008620A CN 200810300862 A CN200810300862 A CN 200810300862A CN 101254897 A CN101254897 A CN 101254897A
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Abstract
The invention discloses a method for preparing titanium hydride and relates to a metal smelting technology field. The method includes mixing titanium material containing titanium oxide, calcium titanate or lithium titanate with the magnesium metal under the calcium or lithium-contained condition; placing into a sealed container, introducing hydrogen and heating to carry out hydrogenation to convert titanium in reaction material into titanium hydride; and removing impurities with acid to obtain titanium hydride. Compared with the prior art, the method has the advantages of greatly reduced comprehensive energy consumption, and process cost reduced by more than 20%, and is applicable to industrial production.
Description
Technical field
The present invention relates to the Metal smelting technical field, particularly a kind of method for preparing titanium hydride.
Technical background
Directly hydrogenation reaction acquisition at high temperature of titanium metal powder is mainly adopted in the preparation of existing titanium hydride, because the difficulty that these metal-powders itself obtain is bigger, therefore cost an arm and a leg, produce with existing production method that the titanium hydride energy consumption is big, cost is higher, be not suitable for the production of industrial mass, therefore limited the application of titanium hydride.
Summary of the invention
Problem to be solved by this invention provides that a kind of technology cost is low, the preparation method of the titanium hydride that is suitable for industrial applications.
For addressing the above problem, the preparation method of titanium hydride of the present invention, it is mixed with MAGNESIUM METAL under the condition that contains calcium or lithium by titanium material, insert in the encloses container and to feed hydrogen and heat and carry out hydrogenation, make the titanium in the reaction mass transform into titanium hydride, will react gains then and other impurity dissolving eccysis beyond the titanium hydride be obtained titanium hydride with acid; Described titanium material includes any in the middle of the titanium oxide, calcium titanate, lithium titanate at least, also can be that these three kinds of materials are planted the mixtures of being formed arbitrarily.
If not calcic or lithium in the titanium material of above-mentioned hydrogenation, or the amount of contained calcium, lithium is not enough, can increase the additive that includes calcium or lithium, the material that can be used as this additive includes any in calcium oxide, calcium hydroxide, lime carbonate, lithium hydroxide, the Quilonum Retard at least, also can be the mixture that their any kind is formed, its objective is the calcium or the lithium that replenish in the described hydrogenation.The amount of required calcium and lithium in the above-mentioned hydrogenation material, the converted weight A that generally gets calcium and lithium is more than 10% of titanium weight summation, described converted weight A=B+3C, B wherein is the weight summation of calcium in the described hydrogenation material, and C wherein is the weight summation of lithium in the described hydrogenation material.Above-mentioned hydrogenation has under the situation of additive in adding, when reaction mass contains water, hydroxide radical, carbonate, can with described titanium material with mix and add hydrogen again with MAGNESIUM METAL after described additive mixes calcination earlier and carry out hydrogenation, the temperature of its calcination generally is 700 ℃～850 ℃, the time of calcination is definite according to the degree that contains water, hydroxide radical, carbonate, is generally to get final product in 1～2 hour; The temperature of described hydrogenation is generally 680 ℃～850 ℃, and the time of described hydrogenation inhales the hydrogen phenomenon according to reaction and stops to determine, is generally 0.5～3 hour.
Embodiment
The invention will be further described below in conjunction with specific embodiment:
Preparation method's 16 examples of titanium hydride:
1, kind and the consumption of determining titanium material according to the facility and the equipment situation of raw material acquisition.
2, select additive for use, is that the principle 10% or more of titanium weight summation is chosen respectively the amount of substance as additive according to the material of selecting different titanium materials and additive by the converted weight A of calcium in the hydrogenation and lithium, converted weight A=B+3C, B wherein is the weight summation of calcium in the hydrogenation material, and C wherein is the weight summation of lithium in the hydrogenation material.
3, be converted into the consumption and excessive 10% that magnesium oxide is determined MAGNESIUM METAL with the oxygen that participates in the reaction mass.
4, selected titanium material (in non-additive embodiment) or selected titanium material and additive mixing (having among the embodiment of additive) place container, calcination postcooling in air;
5, cooled titanium material, additive (in the embodiment of additive is arranged) are crushed to by 100 mesh standard sieves, and be placed in the encloses container with the metal magnesium powder mixing, hydrogen is got rid of, fed to air in the encloses container heat and reduce hydrogenation, reaction is finished back question response product and is chilled to the normal temperature taking-up;
6, after progressively adding reaction product in the entry, the acidity of liquid is transferred to ph=1 with acid, stirring reaction 1 hour, more after filtration, the washing back is with being lower than 80 ℃ hot-air seasoning to constant weight, promptly obtains the titanium hydride finished product.
Material and concrete processing parameter selected among each embodiment are as follows:
Indicate: 1, selected titanium material of the various embodiments described above and the additive industrial raw material that all adopts purity 99%.
2, after testing, the finished product hydrogen content all＞1%.
3, owing to handle through calcination, in other embodiments, titanium sesquioxide and three, tetravalence titanium oxide hydrate replacement of titanium dioxide with the equivalent titanium can draw the identical effect with above-mentioned corresponding embodiment, Gu the same application of titanium sesquioxide and three, tetravalence titanium oxide hydrate is given unnecessary details no longer in an embodiment.
Claims (8)
1. the preparation method of a titanium hydride, it is mixed with MAGNESIUM METAL under the condition that contains calcium or lithium by the titanium material that includes titanium oxide or calcium titanate or lithium titanate, insert in the encloses container and to feed hydrogen and heat and carry out hydrogenation, make the titanium in the reaction mass transform into titanium hydride, will react gains then and other impurity dissolving eccysis beyond the titanium hydride be obtained titanium hydride with acid.
2. the preparation method of titanium hydride according to claim 1 is characterized in that: be added with the additive that includes calcium or lithium in the described hydrogenation material.
3. the preparation method of titanium hydride according to claim 2, it is characterized in that: described additive-package contains any in calcium oxide, calcium hydroxide, lime carbonate, lithium hydroxide, the Quilonum Retard.
4. according to the preparation method of claim 2 or 3 described titanium hydrides, it is characterized in that: described titanium material with carry out hydrogenation with MAGNESIUM METAL, hydrogen again after described additive mixes calcination earlier.
5. the preparation method of titanium hydride according to claim 4, it is characterized in that: the temperature that described titanium material and described additive carry out calcination is 700 ℃～850 ℃, and the time is 1～2 hour.
6. according to the preparation method of claim 1,2 or 3 described titanium hydrides, it is characterized in that: in described hydrogenation material, the converted weight A of calcium or lithium is more than 10% of titanium weight summation, described converted weight A=B+3C, B wherein is the weight summation of calcium in the described hydrogenation material, and C wherein is the weight summation of lithium in the described hydrogenation material; The temperature of described hydrogenation is 680 ℃～850 ℃, and the time is 0.5～3 hour.
7. the preparation method of titanium hydride according to claim 4, it is characterized in that: in described hydrogenation material, the converted weight A of calcium or lithium is more than 10% of titanium weight summation, described converted weight A=B+3C, B wherein is the weight summation of calcium in the described hydrogenation material, and C wherein is the weight summation of lithium in the described hydrogenation material; The temperature of described hydrogenation is 680 ℃～850 ℃, and the time is 0.5～3 hour.
8. the preparation method of titanium hydride according to claim 5, it is characterized in that: in described hydrogenation material, the converted weight A of calcium or lithium is more than 10% of titanium weight summation, described converted weight A=B+3C, B wherein is the weight summation of calcium in the described hydrogenation material, and C wherein is the weight summation of lithium in the described hydrogenation material; The temperature of described hydrogenation is 680 ℃～850 ℃, and the time is 0.5～3 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008103008620A CN101254897B (en) | 2008-04-08 | 2008-04-08 | Method for preparing titanium hydride |
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| CN2008103008620A CN101254897B (en) | 2008-04-08 | 2008-04-08 | Method for preparing titanium hydride |
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| CN101254897A true CN101254897A (en) | 2008-09-03 |
| CN101254897B CN101254897B (en) | 2010-07-28 |
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| CN2008103008620A Expired - Fee Related CN101254897B (en) | 2008-04-08 | 2008-04-08 | Method for preparing titanium hydride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771339A (en) * | 2014-02-08 | 2014-05-07 | 宝鸡市泉兴钛业有限公司 | Special high titanium hydride powder for preparing foamed aluminum and preparation method of special high titanium hydride powder |
| CN106744687A (en) * | 2016-12-06 | 2017-05-31 | 安徽工业大学 | A kind of method that use chemical method prepares titanium hydride powders |
| US10611638B2 (en) | 2014-03-21 | 2020-04-07 | Höganäs Ab (Publ) | Process for manufacturing a metal carbide, nitride, boride, or silicide in powder form |
| CN113501716A (en) * | 2021-07-13 | 2021-10-15 | 西安稀有金属材料研究院有限公司 | Preparation method of crack-free zirconium hydride neutron moderating material |
-
2008
- 2008-04-08 CN CN2008103008620A patent/CN101254897B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771339A (en) * | 2014-02-08 | 2014-05-07 | 宝鸡市泉兴钛业有限公司 | Special high titanium hydride powder for preparing foamed aluminum and preparation method of special high titanium hydride powder |
| CN103771339B (en) * | 2014-02-08 | 2016-02-24 | 宝鸡市泉兴钛业有限公司 | A kind of special high titanium hydride powder preparing foamed aluminium and preparation method thereof |
| US10611638B2 (en) | 2014-03-21 | 2020-04-07 | Höganäs Ab (Publ) | Process for manufacturing a metal carbide, nitride, boride, or silicide in powder form |
| CN106744687A (en) * | 2016-12-06 | 2017-05-31 | 安徽工业大学 | A kind of method that use chemical method prepares titanium hydride powders |
| CN106744687B (en) * | 2016-12-06 | 2018-11-27 | 安徽工业大学 | A method of titanium hydride powders are prepared using chemical method |
| CN113501716A (en) * | 2021-07-13 | 2021-10-15 | 西安稀有金属材料研究院有限公司 | Preparation method of crack-free zirconium hydride neutron moderating material |
| CN113501716B (en) * | 2021-07-13 | 2022-11-29 | 西安稀有金属材料研究院有限公司 | Preparation method of crack-free zirconium hydride neutron moderating material |
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| CN101254897B (en) | 2010-07-28 |
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