Apparatus and method for preparing high-purity spherical magnesium and/or high-purity magnesium powder

Abstract

An apparatus and method for preparing high-purity spherical magnesium and/or high-purity magnesium powder are provided. The apparatus includes a vertical furnace body, a heating zone, and a condensing zone, where a periphery of the condensing zone is provided with a first thermal insulation device and a second thermal insulation device sequentially from bottom to top, and each of the first thermal insulation device and the second thermal insulation device is removably arranged; the periphery of the condensing zone is further provided with a liquid cooling device; a gas inlet and a gas outlet are formed in the condensing zone; and an inner wall of the condensing zone is provided with an arrangement structure configured to arrange a collection device. A heating temperature of a material and condensation conditions in the condensing zone are controlled to make an evaporated magnesium vapor condensed on the collection device in the condensing zone.

What is claimed is: 
     
         1 . An apparatus for preparing high-purity spherical magnesium and/or a high-purity magnesium powder, comprising a vertical furnace body, a heating zone, and a condensing zone, wherein the heating zone and the condensing zone are arranged in the vertical furnace body, and the heating zone is located below the condensing zone;
 a periphery of the heating zone is provided with a heating unit;   a periphery of the condensing zone is provided with a first thermal insulation device and a second thermal insulation device sequentially from bottom to top, and each of the first thermal insulation device and the second thermal insulation device is removably arranged;   the periphery of the condensing zone is further provided with a liquid cooling device;   a gas inlet and a gas outlet are arranged in the condensing zone;   an inner wall of the condensing zone is provided with an arrangement structure configured to arrange a collection device.   
     
     
         2 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 1 , further comprising a filtering device removably arranged between the heating zone and the condensing zone. 
     
     
         3 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 2 , further comprising a plurality of collection devices, wherein a width of each of the plurality of collection devices is greater than a half of a diameter of the vertical furnace body and smaller than the diameter of the vertical furnace body, and the plurality of collection devices are staggered on the inner wall of the condensing zone. 
     
     
         4 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 1 , wherein the liquid cooling device comprises a cooling liquid inlet, a cooling liquid outlet, and a cooling pipeline; the cooling liquid outlet is formed at a top of a side wall surface of the vertical furnace body corresponding to the condensing zone; the cooling pipeline is coiled on an outer wall surface of the heating zone and/or the condensing zone; and the cooling liquid inlet is formed at a bottom of the side wall surface of the vertical furnace body corresponding to the heating zone or the condensing zone. 
     
     
         5 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 4 , further comprising: a vacuum pump and a gas storage device, wherein the vacuum pump is connected to the gas outlet through a pipeline and a first control valve, and the gas storage device is connected to the gas inlet through a pipeline, a second control valve, and a flow meter. 
     
     
         6 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 5 , further comprising a control system, wherein the control system comprises a heating control system, a gas control system, and a cooling liquid-circulation system;
 the heating control system is connected to the heating unit and temperature sensors respectively arranged in the heating zone and the condensing zone;   the gas control system is connected to the vacuum pump, the first control valve, the second control valve, and the flow meter;   the cooling liquid-circulation system is connected to a liquid pump configured to make a cooling liquid circularly flow in the liquid cooling device.   
     
     
         7 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 6 , further comprising a crucible arranged in the heating zone. 
     
     
         8 . A method for preparing high-purity spherical magnesium and/or a high-purity magnesium powder with the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 1 , comprising the following steps:
 S 10 , adding crude magnesium or a magnesium ingot to a crucible, placing the crucible in the heating zone, sequentially arranging a filtering device and a plurality of collection devices above the crucible, and sealing the vertical furnace body;   S 20 , turning on a vacuum pump and a first control valve to allow vacuuming; when a vacuum degree in the vertical furnace body reaches a preset vacuum degree, starting to heat the heating zone, and turning on both a second control valve and a cooling liquid-circulation system to make a gas and a cooling liquid flow, wherein the gas is a gas that does not react with a magnesium vapor, and the cooling liquid is a cooling medium of water or oil; and   controlling a temperature of the heating zone at 650° C. to 1,500° C., adjusting a gas flow rate by the second control valve to 1 LPM to 500 LPM, adjusting a cooling liquid flow rate to 1 LPM to 100 LPM, and controlling a temperature of the condensing zone at 100° C. to 700° C.; and   S 30 , when the crude magnesium or the magnesium ingot evaporates completely, stopping the heating; and when a temperature in a furnace drops to room temperature, turning off a gas control system and the cooling liquid-circulation system, and taking the plurality of collection devices out to obtain the high-purity spherical magnesium and/or the high-purity magnesium powder.   
     
     
         9 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 8 , wherein when the temperature of the heating zone is controlled at 650° C. to 900° C., the gas flow rate is adjusted by the second control valve to 200 LPM to 500 LPM, the cooling liquid flow rate is adjusted to 50 LPM to 100 LPM, and the temperature of the condensing zone is controlled at 100° C. to 400° C., the high-purity magnesium powder alone is obtained; when the temperature of the heating zone is controlled at 900° C. to 1,500° C., the gas flow rate is adjusted by the second control valve to 1 LPM to 200 LPM, the cooling liquid flow rate is adjusted to 1 LPM to 50 LPM, and the temperature of the condensing zone is controlled at 400° C. to 700° C., the high-purity spherical magnesium alone is obtained; and when the temperature of the heating zone is controlled at 800° C. to 1,300° C. and preferably 900° C. to 1,200° C., the gas flow rate is controlled at 100 LPM to 400 LPM and preferably 200 LPM and 300 LPM, the cooling liquid flow rate is controlled at 30 LPM to 70 LPM and preferably 40 LPM to 60 LPM, and a temperature of a condensate is controlled at 200° C. to 600° C., both the high-purity spherical magnesium and the high-purity magnesium powder are obtained. 
     
     
         10 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 9 , wherein when the high-purity magnesium powder alone is prepared, the first thermal insulation device and the second thermal insulation device are removed; when the high-purity spherical magnesium alone is prepared, the first thermal insulation device and the second thermal insulation device are arranged; and when both the high-purity spherical magnesium and the high-purity magnesium powder are prepared, the first thermal insulation device is arranged, and the second thermal insulation device is removed. 
     
     
         11 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 2 , wherein the liquid cooling device comprises a cooling liquid inlet, a cooling liquid outlet, and a cooling pipeline; the cooling liquid outlet is formed at a top of a side wall surface of the vertical furnace body corresponding to the condensing zone; the cooling pipeline is coiled on an outer wall surface of the heating zone and/or the condensing zone; and the cooling liquid inlet is formed at a bottom of the side wall surface of the vertical furnace body corresponding to the heating zone or the condensing zone. 
     
     
         12 . The apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 3 , wherein the liquid cooling device comprises a cooling liquid inlet, a cooling liquid outlet, and a cooling pipeline; the cooling liquid outlet is formed at a top of a side wall surface of the vertical furnace body corresponding to the condensing zone; the cooling pipeline is coiled on an outer wall surface of the heating zone and/or the condensing zone; and the cooling liquid inlet is formed at a bottom of the side wall surface of the vertical furnace body corresponding to the heating zone or the condensing zone. 
     
     
         13 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 8 , wherein the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder further comprises the filtering device removably arranged between the heating zone and the condensing zone. 
     
     
         14 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 13 , wherein the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder further comprises the plurality of collection devices, a width of each of the plurality of collection devices is greater than a half of a diameter of the vertical furnace body and smaller than the diameter of the vertical furnace body, and the plurality of collection devices are staggered on the inner wall of the condensing zone. 
     
     
         15 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 8 , wherein the liquid cooling device comprises a cooling liquid inlet, a cooling liquid outlet, and a cooling pipeline; the cooling liquid outlet is formed at a top of a side wall surface of the vertical furnace body corresponding to the condensing zone; the cooling pipeline is coiled on an outer wall surface of the heating zone and/or the condensing zone; and the cooling liquid inlet is formed at a bottom of the side wall surface of the vertical furnace body corresponding to the heating zone or the condensing zone. 
     
     
         16 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 15 , wherein the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder further comprises the vacuum pump and a gas storage device, wherein the vacuum pump is connected to the gas outlet through a pipeline and the first control valve, and the gas storage device is connected to the gas inlet through a pipeline, the second control valve, and a flow meter. 
     
     
         17 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 16 , wherein the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder further comprises a control system, wherein the control system comprises a heating control system, the gas control system, and the cooling liquid-circulation system;
 the heating control system is connected to the heating unit and temperature sensors respectively arranged in the heating zone and the condensing zone;   the gas control system is connected to the vacuum pump, the first control valve, the second control valve, and the flow meter;   the cooling liquid-circulation system is connected to a liquid pump configured to make a cooling liquid circularly flow in the liquid cooling device.   
     
     
         18 . The method for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder according to  claim 17 , wherein the apparatus for preparing the high-purity spherical magnesium and/or the high-purity magnesium powder further comprises the crucible arranged in the heating zone.