CN102001626A - Method and device for preparing superfine zirconium hydride powder by continuous dynamic hydrogenation method - Google Patents
Method and device for preparing superfine zirconium hydride powder by continuous dynamic hydrogenation method Download PDFInfo
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- CN102001626A CN102001626A CN 201010545076 CN201010545076A CN102001626A CN 102001626 A CN102001626 A CN 102001626A CN 201010545076 CN201010545076 CN 201010545076 CN 201010545076 A CN201010545076 A CN 201010545076A CN 102001626 A CN102001626 A CN 102001626A
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Abstract
The invention relates to a method and a device for preparing superfine zirconium hydride (ZrH2) powder by a continuous dynamic hydrogenation method, and belongs to the technical field of metal hydride materials. The method is characterized by comprising the following steps of: putting sponge zirconium or metal zirconium scraps into a stocker, and vacuumizing so as to dehydrate the sponge zirconium; heating a dynamic steel tube when the vacuum is 3*10<-2> to 7*10<-2>Pa, closing a vacuum valve and a vacuum system and introducing high-purity H2 into the steel tube when the temperature is between 550 and 650 DEG C, and simultaneously conveying the sponge zirconium into a rotating thermal steel tube at a rate of 3 to 5kg/h so as to hydrogenate the sponge zirconium at the rotating speed of 30 to 50 revolutions per minute, wherein the flow of the hydrogen is 0.5 to 3L/S; standing the sponge zirconium in a heating area so as to ensure that the sponge zirconium is hydrogenated into a subsaturation state, and conveying the sponge zirconium to an air-cooled area for continuous hydrogenating for 0.3 to 1 hour; and feeding into a water-cooled jacket area, and feeding the sponge zirconium into a vacuum receiving device for performing primary crushing and roller-milling and ball-milling refining so as to prepare the superfine zirconium hydride powder. The device contributes to reaction of the hydrogen and the sponge zirconium, contributes to preparing the superfine ZrH2 powder and can realize continuous production of the zirconium hydride powder.
Description
Technical field
The present invention relates to a kind of ultra-fine zircoium hydride (ZrH that under dynamic environment, prepares
2) method and the device thereof of powder, this method helps the reaction of hydrogen and zirconium sponge or metal zirconium chip, and hydrogenation and ZrH reach capacity
2Hold broken up characteristics, help preparing ultra-fine ZrH
2Powder.The technical field that belongs to metal hydride material.
Background technology
ZrH
2Being a kind of metal hydride of excellence, is one of main target of neutron tube, and number of hydrogen atoms density wherein is up to 7.3 * 10
22Cm
-3Adopt the target of the hydride of zirconium, can obtain a large amount of neutrons as neutron tube; Simultaneously, ZrH
2In thermobattery and pyrotechnics industrial additive, also obtain very big application.
The method for preparing at present the zircoium hydride powder is to use the static hydrogen method, there be being deposited in the hydrogen environment of zirconium sponge or metal zirconium chip static state in this method, hydrogen and zirconium contact area under static state is lower, hinder hydrogen to internal diffusion, exist zirconium sponge or metal zirconium chip not thorough in hydrogenation process; Zirconium sponge or metal zirconium chip and hydrogen reaction are exothermic reactions simultaneously, if zirconium sponge or metal zirconium chip are piled up overlong time under thermal environment, cause hydrogenated products to sinter ZrH into easily
2Caking, the difficulty or ease fragmentation, the production efficiency that can't prepare out ultra-fine zircoium hydride powder or zircoium hydride powder is lower, has restricted the production of high-quality ultra-fine fine zircoium hydride.
Summary of the invention
The purpose of this invention is to provide a kind of dynamic method and prepare ultra-fine ZrH
2The method of powder and device thereof.The objective of the invention is in its reaction process, to utilize the motion of material to increase the chance that hydrogen contacts with material, increase the reaction area of zirconium sponge or metal zirconium chip and hydrogen, a large amount of heats of zirconium sponge or metal zirconium chip and hydrogen generation can be passed through the rapid radiation refrigeration of motion system simultaneously, prevent that hydrogenated products from sintering ZrH into
2Caking reaches efficient and ultralow hydrogenant purpose.
A kind of dynamic method of the present invention prepares ultra-fine ZrH
2The method of powder and device thereof, it is characterized in that adopting zirconium sponge or metal zirconium chip is raw material, it is contained in (steel pipe can rotate) in the rotary heating, vacuum steel tube under the control of motor, under dynamic hot hydrogen environment, reach the purpose that efficient hydrogenation and reaction product are not easy to lump.
The present invention adopts following technical scheme:
Dynamically hydride process prepares ultra-fine zircoium hydride ZrH continuously
2The method of powder:
(1), store holder, material feeder, heating zone, air cooling zone and water-cooled district are vacuumized the moisture removal that makes in zirconium sponge or the metal zirconium chip with the 0.5-10kg zirconium sponge or clean up air dried metal zirconium chip and put into store holder;
(2) reach 3 * 10 when vacuum
-2~ 7 * 10
-2p
aThe time, give dynamic steel pipe heating with NiCr silk heating element stove, when temperature reaches 550 ~ 650 ℃, close vacuum valve and vacuum system, in steel pipe, begin to feed high-purity H
2, to give simultaneously in the hot steel pipe that rotates and carry zirconium sponge or metal zirconium chip to make its hydrogenation with 3-5Kg/h, the rotating speed of steel pipe is 30-50 commentaries on classics/min, the flow of hydrogen flows in the stove with 0.5 ~ 3L/S (i.e. liter/second);
(3) because Zr+H
2=ZrH
2It is thermopositive reaction, system temperature sharply rose to 850 ~ 900 ℃ after zirconium was inhaled hydrogen in a large number, and it is favourable continuously in the carrying out that inhales hydrogen to reduce system temperature, the system temperature scope is suitably controlled the suction hydrogen speed that to control titanium sponge, in order to keep system temperature at 550 ~ 650 ℃, so after in half an hour, when zirconium does not reach capacity hydrogenation, just being sent to air cooling zone at the hydrogenant zirconium continues among the hydrogenase 10 .3-1h, this moment, zirconium was by saturated hydrogenation, the steel pipe rotation is sent saturated zircoium hydride into the water jacket district, sends into then in the vacuum collector and stores, and collector can be stored the ZrH of 50Kg
2In the vacuum collector, carry out just fragmentation, barreling and ball milling refinement, obtain ultra-fine ZrH
2Powder.
Dynamically hydride process prepares ultra-fine ZrH continuously
2The device of powder, promptly dynamic hydrogenation apparatus, this device comprise store holder, hydrogen cylinder and pipeline thereof, material feeder, dynamic steel pipe, temperature and speed control system, vacuum collector, surplus hydrogen burning mouth.Store holder stores zirconium sponge or metal zirconium chip; Hydrogen cylinder and pipeline thereof link to each other with material feeder, are used to provide raw hydrogen; Material feeder utilization motor rotating pulley is given in the dynamic steel pipe of heating zone and is sent zirconium sponge or metal zirconium chip continuously; Dynamically steel pipe can be divided into heating zone, three parts of air cooling zone and water-cooled district, and the heating zone is used for making ZrH
2, air cooling zone and water-cooled district are used for cooling off ZrH
2Dynamically an end of steel pipe links to each other with material feeder, and the other end links to each other with the vacuum collector, and store holder, pumped vacuum systems and hydrogen cylinder and pipeline thereof link to each other with material feeder respectively; Temperature and speed control system are used for controlling the temperature of heating and the rotating speed of dynamic steel pipe; The vacuum collector is used to store the ZrH for preparing
2Discharge port is used for ZrH
2Collection; Surplus hydrogen burning mouth is used to fail the processing of hydrogen of complete reaction.Motor links to each other with dynamic steel pipe, drives the rotation of steel pipe by the rotation of motor, thereby realizes ZrH
2Moving of steel duct; Temperature and speed control system be positioned at dynamic steel pipe below, by control motor velocity of rotation control ZrH
2Translational speed, control the temperature of heating zone by the power of control NiCr silk heating element stove.
Characteristics of the present invention are: dynamic this part of steel pipe.This device is because the existence of dynamic steel pipe has realized ZrH
2Continuity production.ZrH in the heating zone preparation
2, move to air cooling zone by the rotation of steel pipe, further rotate and enter the water-cooled district, enter the vacuum collector at last, collect ZrH by discharge port
2, all production processes all are successive.This device can be realized ZrH
2Continuity production.
This dynamic method prepares ultra-fine ZrH
2In the used isolated plant of powder, described heat resisting pipe thickness of pipe is 3mm; Material is a 1Cr5Mo high temperature steel.
Description of drawings
Fig. 1 is the rough schematic of the inventive method isolated plant.
Each numeral is as follows among the figure:
1, material feeder 2, store holder 3, pumped vacuum systems 4, heating zone 5, air cooling zone 6, water-cooled district 7, vacuum collector 8, surplus hydrogen burning mouth 9, discharge port 10, temperature and speed control system 11, hydrogen cylinder and pipeline 12 thereof, motor.
Embodiment
After now embodiments of the invention specifically being described in.
This present invention's continuously dynamic hydride process prepares ultra-fine ZrH
2The method of powder adopts and cleans up air dried metal zirconium chip is raw material, makes its hydrogenation under dynamic environment at feeding high-purity hydrogen under vacuum and the thermal environment, realizes efficient saturated hydrogenant purpose.
The isolated plant that this method is used, as shown in Figure 1, this device includes material feeder (utilization motor rotating pulley is that steel pipe send zirconium sponge or metal zirconium chip continuously to heating) 1, store holder (storing zirconium sponge or metal zirconium chip) 2, pumped vacuum systems 3, [motor can drive steel pipe and rotate dynamic steel pipe, runs through the heating zone and (generates ZrH
2) 4, air cooling zone (cooling reaction product ZrH
2) 5, water-cooled district (cooling reaction product ZrH
2) 6], the vacuum collector (collects ZrH
2Product) 7.NiCr silk heating element process furnace (being positioned at the heating zone) can heat for the part that dynamic steel pipe is positioned at the heating zone, and the height of Heating temperature can be controlled.With pumped vacuum systems 3 is earlier that material feeder 1, store holder 2, heating zone 4, air cooling zone 5, water-cooled district 6, vacuum collector 7 systems vacuumize, when vacuum tightness reaches 3 * 10
-2~ 7 * 10
-2During pa, give dynamic steel pipe heating, when temperature reaches 550 ~ 650 ℃, close vacuum valve and vacuum system, in dynamic steel pipe, begin to feed high-purity H with NiCr silk heating element stove
2Open the valve of material feeder 1 simultaneously, giving in the dynamic steel pipe carries zirconium sponge or metal zirconium chip to make its hydrogenation with 3-5Kg/h, dynamically the rotating speed of steel pipe is 30-50 commentaries on classics/min, and the flow of hydrogen is 0.5 ~ 3L/S, behind 0.5 ~ 2h, when zirconium does not reach capacity hydrogenation, to just deliver to air cooling zone 5 and continue hydrogenase 10 .2 ~ 1.5h, then saturated zircoium hydride be sent into water-cooled district 6, send into vacuum collector 7 at last at the hydrogenant zirconium.In vacuum collector 7, carry out just broken 0.3h ~ 3h and barreling 0.3h ~ 3h, after efficient ball milling refinement 0.3h ~ 4h obtains ultra-fine ZrH
2Powder.
Described heat resisting pipe thickness of pipe is 3mm; Material is a 1Cr5Mo high temperature steel.
The operating process of this enforcement is as follows:
Embodiment 1
To clean up the air dried 1kg metal zirconium chip store holder 2 of packing into, be earlier that material feeder 1, store holder 2, heating zone 4, air cooling zone 5, water-cooled district 6, vacuum collector 7 systems vacuumize with pumped vacuum systems 8, when vacuum tightness reaches 4.5 * 10 then
-2During pa,, close vacuum valve and vacuum system, in dynamic steel pipe, begin to feed high-purity H with the heating zone part Heating temperature to 600 ℃ that NiCr silk heating element stove is given dynamic steel pipe
2The flow of hydrogen is 0.8L/S, dynamically the rotating speed of steel pipe is 35 commentaries on classics/min, open the valve of material feeder 1 simultaneously, giving in the dynamic steel pipe carries zirconium sponge or metal zirconium chip to make its hydrogenation with 3Kg/h, dynamically the rotating speed of steel pipe is 35 commentaries on classics/min, the flow of hydrogen flows in the stove with 0.8L/S, the zirconium chip is after the heating zone stops 0.7h, be hydrogenated and be half saturated zircoium hydride, to just deliver to air cooling zone 5 then and continue hydrogenase 10 .4h, saturated zircoium hydride will be sent into water-cooled district 6, send into vacuum collector 7 at last at the hydrogenant zirconium.Carry out just broken 0.5h and barreling 2h at vacuum collector 7, after efficient ball milling refinement 2h, obtaining granularity is the ultra-fine ZrH of 2um
2Powder.
Concrete technology is as follows: the zirconium sponge → dynamically hydrogenation → fragmentation → barreling just → efficient ultra-fine ZrH of ball milling refinement → 2um
2Powder.
Embodiment 2
To clean up the air dried 2kg metal zirconium chip store holder of packing into, be earlier that material feeder 1, store holder 2, heating zone 4, air cooling zone 5, water-cooled district 6, vacuum collector 7 systems vacuumize with pumped vacuum systems 8, when vacuum tightness reaches 6 * 10 then
-2During pa, give dynamic steel pipe Heating temperature to 620 ℃, close vacuum valve and vacuum system, in dynamic steel pipe, begin to feed high-purity H with NiCr silk heating element stove
2The flow of hydrogen is 1.0L/S, dynamically the rotating speed of steel pipe is 40 commentaries on classics/min, open the valve of material feeder 1 simultaneously, giving in the dynamic steel pipe carries zirconium sponge or metal zirconium chip to make its hydrogenation with 4Kg/h, dynamically the rotating speed of steel pipe is 40 commentaries on classics/min, the flow of hydrogen flows in the stove with 1.0L/S, the zirconium chip is after the heating zone stops 0.6h, be hydrogenated and be half saturated zircoium hydride, to just deliver to air cooling zone 5 then and continue hydrogenase 10 .5h, saturated zircoium hydride will be sent into water-cooled district 6, send into vacuum collector 7 at last at the hydrogenant zirconium.Carry out just broken 0.7h and barreling 2.5h at vacuum collector 7, after efficient ball milling refinement 2.2h, obtaining granularity is the ultra-fine ZrH of 1.5um
2Powder.
Claims (2)
- One kind continuously dynamically hydride process prepare the method for ultra-fine zircoium hydride powder, it is characterized in that this method has following processing step:With zirconium sponge or clean up air dried metal zirconium chip and put into store holder, store holder, material feeder, heating zone, air cooling zone and water-cooled district are vacuumized the moisture removal that makes in zirconium sponge or the metal zirconium chip;When vacuum reaches 3 * 10 -2~ 7 * 10 -2P aThe time, give dynamic steel pipe heating, when temperature reaches 550 ~ 650 ℃, close vacuum valve and vacuum system, in steel pipe, begin to feed high-purity H 2, to give simultaneously in the hot steel pipe that rotates and carry zirconium sponge or metal zirconium chip to make its hydrogenation with 3 ~ 5Kg/h, the rotating speed of steel pipe is 30 ~ 50 commentaries on classics/min, the flow of hydrogen is 0.5 ~ 3L/S;Zirconium sponge or metal zirconium chip stop after be hydrogenated to semi-saturation in the heating zone, be sent to air cooling zone and continue hydrogenase 10 .3 ~ 1h, send into the water jacket district then, send into again and carry out just fragmentation, barreling and ball milling refinement in the vacuum collector, obtain ultra-fine zircoium hydride powder.
- 2. one kind is used for the device that the described continuously dynamic hydride process of claim 1 prepares ultra-fine zircoium hydride powder method, this device is by material feeder (1), store holder (2), pumped vacuum systems (3), dynamic steel pipe, vacuum collector (7), temperature and speed control system (10) and hydrogen cylinder and pipeline (11) thereof are formed, it is characterized in that: dynamically steel pipe is divided into heating zone (4), (6) three parts in air cooling zone (5) and water-cooled district, dynamically an end of steel pipe links to each other with material feeder (1), the other end links to each other with vacuum collector (7), store holder (2), pumped vacuum systems (3) links to each other with material feeder (1) respectively with hydrogen cylinder and pipeline (11) thereof; Temperature and speed control system (10) are controlled the temperature of heating zone (4) by the power of control NiCr silk heating element stove, motor (12) links to each other with dynamic steel pipe, and temperature and speed control system (10) are controlled the translational speed of zircoium hydride in dynamic steel pipe by the velocity of rotation of control motor (12).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105450764A CN102001626B (en) | 2010-11-16 | 2010-11-16 | Method and device for preparing superfine zirconium hydride powder by continuous dynamic hydrogenation method |
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|---|---|---|---|
| CN2010105450764A CN102001626B (en) | 2010-11-16 | 2010-11-16 | Method and device for preparing superfine zirconium hydride powder by continuous dynamic hydrogenation method |
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| CN102001626B CN102001626B (en) | 2012-02-15 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045058A (en) * | 2014-07-01 | 2014-09-17 | 昆明冶金研究院 | Device and method for preparing non-caking unsaturated hydride controllable in hydrogen content |
| CN104107917A (en) * | 2014-07-18 | 2014-10-22 | 中信锦州金属股份有限公司 | Method for producing ultrafine zirconium powder |
| CN104289709A (en) * | 2014-10-31 | 2015-01-21 | 中南大学 | Preparation method for superfine zirconium powder |
| CN110773750A (en) * | 2019-12-16 | 2020-02-11 | 重庆优钛新材料科技有限公司 | Method and device for preparing high-purity superfine metal powder |
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| CN1789455A (en) * | 2004-12-15 | 2006-06-21 | 北京有色金属研究总院 | Hydrogen compression material of metal hydride |
| CN101559926A (en) * | 2008-04-17 | 2009-10-21 | 北京有色金属研究总院 | Method for preparing zirconium hydride |
| CN101254898B (en) * | 2008-04-08 | 2010-10-27 | 李健民 | Method for preparing zirconium hydride |
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2010
- 2010-11-16 CN CN2010105450764A patent/CN102001626B/en not_active Expired - Fee Related
Patent Citations (5)
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| GB1085854A (en) * | 1964-08-26 | 1967-10-04 | Degussa | A process for the production of titanium, zirconium or thorium hydride |
| JPH10158001A (en) * | 1996-11-29 | 1998-06-16 | Mitsubishi Materials Corp | Production of zirconium hydride |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045058A (en) * | 2014-07-01 | 2014-09-17 | 昆明冶金研究院 | Device and method for preparing non-caking unsaturated hydride controllable in hydrogen content |
| CN104107917A (en) * | 2014-07-18 | 2014-10-22 | 中信锦州金属股份有限公司 | Method for producing ultrafine zirconium powder |
| CN104107917B (en) * | 2014-07-18 | 2016-07-06 | 中信锦州金属股份有限公司 | A kind of production method of ultra fine Zr powder |
| CN104289709A (en) * | 2014-10-31 | 2015-01-21 | 中南大学 | Preparation method for superfine zirconium powder |
| CN110773750A (en) * | 2019-12-16 | 2020-02-11 | 重庆优钛新材料科技有限公司 | Method and device for preparing high-purity superfine metal powder |
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