CN1718788A - Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor - Google Patents
Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor Download PDFInfo
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- CN1718788A CN1718788A CN 200510003109 CN200510003109A CN1718788A CN 1718788 A CN1718788 A CN 1718788A CN 200510003109 CN200510003109 CN 200510003109 CN 200510003109 A CN200510003109 A CN 200510003109A CN 1718788 A CN1718788 A CN 1718788A
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Abstract
A process for using titanium hydride powder to titanize the inner surface of the new reactor used for preparing spongy iron includes such steps as testing leakage, immersing in acid, water washing, baking uniformly coating a powdered titanium hydride layer, putting it in heater, vacuum dehydrogenating at 150-250 deg.C for 2-5hr, medium-temp dehydrogenating by three temp levels for 1-2 hr for each temp level, filling inertial gas, high-temp sinter at 960-980 deg.C for 8-15 hr, and cooling.
Description
Technical field
The invention belongs to the non-ferrous metal technical field, the New Development of particularly a kind of titanium sponge reduction, distillation production usefulness is answered the method for using the hydride powder titanizing titanium in the device.
Background technology
Employed new reactor is produced in titanium sponge reduction, distillation, generally adopts plain carbon stool to make.For the iron rust that prevents the inner wall of new reactor surface and iron at high temperature enter during titanium sponge sticks together, must ooze titanium to the inner wall surface of new reactor before using, just can guarantee the quality product of extra large bright and beautiful titanium.New Development is answered device to ooze titanium required titanium valve granularity and internal soundness and is had relatively high expectations, and the particle size diameter general requirement is not more than 0.043mm.
The conventional titanium valve titanizing method that uses, be with new reactor through acidleach, wash, dry up after, wall surface is inserted in the heating installation after being coated with and brushing certain fine-grained titanium valve more within it, and through the low temperature degassing, high-temperature sintering process, makes titanium valve stick to the inner wall surface of new reactor.Be difficult for to obtain owing to ooze the required titanium valve of titanium, when especially sieving fine-grained titanium valve, labour intensity and spillage of material are big, the cost height, and also titanium valve is when screening, and easily by oxygen, polluted by nitrogen, the titanium valve particle of screening is inhomogeneous, flowability and poor adhesion.
Summary of the invention
The objective of the invention is at using titanium valve to ooze the problems that titanium exists in the above-mentioned new reactor, a kind of interior method of using the hydride powder titanizing titanium of new reactor of producing titanium sponge is provided.The titanium hydride powder cost that this method is used is low, uniform particles, and flowability and adhesivity are strong, and it is effective to ooze titanium.
The new reactor that the inventive method is used must be after leak detection, acidleach, washing, dry up the link processing, the inner wall surface layer of new reactor equably brushing thickness be that 0.08～0.5 millimeter, particle size diameter is not in the titanium hydride powder of 0.043mm, new reactor after will brushing is again inserted in the heating installation, outgases through 2～5 hours 150～250 ℃ of low temperature under vacuum.After the low temperature degassing finishes, then through in warm dehydrogenation, its temperature is controlled to be 250～350 ℃, 350～550 ℃, 550～700 ℃ three constant temperature zones according to first latter stage, and each constant temperature 1～2 hour.Dehydrogenation finishes back input rare gas element, again through 8～15 hours high temperature sinterings of 960～980 ℃.High temperature sintering finishes the back and takes out, and inserts in the water cooler and cools off, and promptly finishes the titanium that oozes of the present invention.
Titanizing method cost of the present invention is low, its uniform particles, and flowability and adhesivity are strong, and it is effective to ooze titanium, thereby guarantees the titanium products quality of sponge.
Embodiment
The new reactor that the inventive method is used must be through leak detection, hunt leak qualified after, carry out pickling, promptly adopt diluted technical hydrochloric acid that new reactor was soaked 7～10, remove the greasy dirt, oxidation iron rust on inner wall of new reactor surface etc., reach titanium hydride powder can directly be adsorbed on the inner wall surface that is bonded in new reactor.Acid is carried out Xian clearly with high pressure water behind Xian, and the sour water and the foul on inner wall of new reactor surface washed away, and is as the criterion up to exposing metallic surface gloss.The pressurized air of washing back Yong Chun Net dries up inner wall of new reactor.Before oozing titanium, each link processing quality of new reactor will directly have influence on oozes the titanium quality.
New reactor by leak detection, acidleach, wash, dry up link after, use titanium hydride powder to replace titanium valve to ooze titanium.When selecting titanium hydride powder, its carbon content should be not more than 0.04%, hydrogen is not more than 0.06%, silicon is not more than 0.02%, iron is not more than 0.10%, chlorine is not more than 0.06%.The titanium hydride powder that particle size diameter is not more than 0.043mm is brushed the inner wall surface at new reactor equably, and its thickness is 0.08～0.5 millimeter, and being coated with the titanium hydride powder that brushes must not the group of rising and flow.Insert in time in the process furnace after will oozing big lid that titanium uses and new reactor assembling, after new reactor is got rid of aqueous vapor through finding time, under vacuum,, separate out remaining hydrogen chloride gas and aqueous vapor in the new reactor through 150～250 ℃ of low temperature degassings in 2～5 hours.After the low temperature degassing, then through in warm dehydrogenation, its temperature is controlled to be 250～350 ℃, 350～550 ℃, 550～700 ℃ three constant temperature zones according to first latter stage, and each constant temperature 1～2 hour, and the hydrogen in the titanium hydride powder is sloughed.The titanium valve of sloughing hydrogen has active very strong newborn titanium atom, is easier to bonding.Dehydrogenation finishes back input rare gas element to be protected, and again through 8～15 hours high temperature sinterings of 960～980 ℃, makes titanium hydride powder stick to the inner wall surface of new reactor through high temperature sintering.High temperature sintering finishes the back and takes out, and inserts in the water cooler and cools off.After cooling, the air pressure in the new reactor is higher than barometric point 0.005～0.03MPa, reaches the purpose that prevents in the air admission new reactor, promptly finishes the titanium that oozes of the present invention.The inventive method is oozed the titanium sponge product that the new reactor behind the titanium is produced, its iron contamination, hydrogen foreign matter content average out to 0.045% and 0.0014%, and the iron contamination, the hydrogen foreign matter content that ooze the titanium sponge product of the new reactor production behind the titanium than titanium valve lack.
Claims (4)
1, a kind of by leak detection, acidleach, wash, dry up the method for using the hydride powder titanizing titanium in the new reactor that the back produces titanium sponge, it is characterized in that with the inner wall surface layer of new reactor equably brushing thickness be the titanium hydride powder that 0.08～0.5 millimeter, particle size diameter are not more than 0.043mm, again new reactor is inserted in the heating installation, under vacuum, outgas through low temperature, then warm dehydrogenation in the warp, dehydrogenation finishes back input rare gas element, again through high temperature sintering, high temperature sintering finishes the back and takes out, and inserts in the water cooler and cools off.
2, it is 2～5 hours that titanizing method according to claim 1, the temperature that it is characterized in that the low temperature degassing are controlled to be 150～250 ℃, time.
3, titanizing method according to claim 1, the temperature of warm dehydrogenation is controlled to be 250～350 ℃, 350～550 ℃, 550～700 ℃ three constant temperature zones according to first latter stage in it is characterized in that, and each constant temperature 1～2 hour.
4, titanizing method according to claim 1 is characterized in that the temperature of high temperature sintering is controlled to be 960～980 ℃, and the time is 8～15 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510003109 CN1283829C (en) | 2005-06-17 | 2005-06-17 | Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510003109 CN1283829C (en) | 2005-06-17 | 2005-06-17 | Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor |
Publications (2)
| Publication Number | Publication Date |
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| CN1718788A true CN1718788A (en) | 2006-01-11 |
| CN1283829C CN1283829C (en) | 2006-11-08 |
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| CN 200510003109 Expired - Fee Related CN1283829C (en) | 2005-06-17 | 2005-06-17 | Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912972A (en) * | 2010-08-05 | 2010-12-15 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN101676431B (en) * | 2008-09-18 | 2012-02-01 | 朝阳百盛锆钛股份有限公司 | Method for titanizing inner wall of new reactor in production of titanium sponge |
| EA018035B1 (en) * | 2009-10-07 | 2013-05-30 | Компания Адма Продактс, Инкорпорейтед | Method for manufacturing articles from titanium alloys |
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| JP2020002435A (en) * | 2018-06-28 | 2020-01-09 | 東邦チタニウム株式会社 | Manufacturing method of metallic reduction reaction vessel, metallic reduction reaction vessel, and manufacturing method of titanium |
| JP2020002434A (en) * | 2018-06-28 | 2020-01-09 | 東邦チタニウム株式会社 | Manufacturing method of metallic reduction reaction vessel including diffusion layer, manufacturing method of high melting point metal, and coating material for metallic reduction reaction vessel |
| CN111118309A (en) * | 2020-03-19 | 2020-05-08 | 遵义钛业股份有限公司 | Device and method for titanizing large cover in titanium sponge production |
| CN111378921A (en) * | 2020-05-18 | 2020-07-07 | 攀钢集团钛业有限责任公司 | Titanizing method and titanizing agent for inner wall of titanium sponge stainless steel reactor |
| CN113584325A (en) * | 2021-06-21 | 2021-11-02 | 洛阳双瑞万基钛业有限公司 | Repair method for titanium infiltration layer of reactor in production process of titanium sponge |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691649B (en) * | 2009-09-25 | 2011-05-11 | 朝阳金达钛业有限责任公司 | Titanizing and aluminizing method for sponge titanium reactor |
| CN102953029A (en) * | 2011-08-26 | 2013-03-06 | 攀钢集团有限公司 | Surface treatment method for titanium sponge reactor |
-
2005
- 2005-06-17 CN CN 200510003109 patent/CN1283829C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676431B (en) * | 2008-09-18 | 2012-02-01 | 朝阳百盛锆钛股份有限公司 | Method for titanizing inner wall of new reactor in production of titanium sponge |
| EA018035B1 (en) * | 2009-10-07 | 2013-05-30 | Компания Адма Продактс, Инкорпорейтед | Method for manufacturing articles from titanium alloys |
| CN101912972A (en) * | 2010-08-05 | 2010-12-15 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN101912972B (en) * | 2010-08-05 | 2011-12-28 | 成都韵智科技有限公司 | Preparation method of superfine Ti powders |
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| JP2020002434A (en) * | 2018-06-28 | 2020-01-09 | 東邦チタニウム株式会社 | Manufacturing method of metallic reduction reaction vessel including diffusion layer, manufacturing method of high melting point metal, and coating material for metallic reduction reaction vessel |
| JP2020002435A (en) * | 2018-06-28 | 2020-01-09 | 東邦チタニウム株式会社 | Manufacturing method of metallic reduction reaction vessel, metallic reduction reaction vessel, and manufacturing method of titanium |
| JP7106371B2 (en) | 2018-06-28 | 2022-07-26 | 東邦チタニウム株式会社 | METHOD FOR MANUFACTURING METAL REDUCTION REACTION VESSEL WITH DIFFUSION LAYER, METHOD FOR MANUFACTURE OF HIGH-MELTING METAL, AND COATING MATERIAL FOR METAL REDUCE REACTION VESSEL |
| JP7106372B2 (en) | 2018-06-28 | 2022-07-26 | 東邦チタニウム株式会社 | METHOD FOR MANUFACTURING METAL REDUCTION REACTION VESSEL, METHOD FOR MANUFACTURING METAL REDUCTION REACTION VESSEL, AND TITANIUM |
| CN111118309A (en) * | 2020-03-19 | 2020-05-08 | 遵义钛业股份有限公司 | Device and method for titanizing large cover in titanium sponge production |
| CN111378921A (en) * | 2020-05-18 | 2020-07-07 | 攀钢集团钛业有限责任公司 | Titanizing method and titanizing agent for inner wall of titanium sponge stainless steel reactor |
| CN111378921B (en) * | 2020-05-18 | 2022-07-22 | 攀钢集团钛业有限责任公司 | Titanizing method and titanizing agent for inner wall of titanium sponge stainless steel reactor |
| CN113584325A (en) * | 2021-06-21 | 2021-11-02 | 洛阳双瑞万基钛业有限公司 | Repair method for titanium infiltration layer of reactor in production process of titanium sponge |
| CN113584325B (en) * | 2021-06-21 | 2022-07-19 | 洛阳双瑞万基钛业有限公司 | Repair method for titanium infiltration layer of reactor in production process of titanium sponge |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1283829C (en) | 2006-11-08 |
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Application publication date: 20060111 Assignee: Zunyi Boyu Titanium Co., Ltd. Assignor: Zunyi Titanium Industry Co., Ltd. Contract record no.: 2012520000016 Denomination of invention: Method of producing sponge titanium by using titanium hydride powder titanizing in new reactor Granted publication date: 20061108 License type: Exclusive License Record date: 20121225 |
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