阅读说明：本技术 一种海绵锆的生产设备及工艺 (Production equipment and process of zirconium sponge ) 是由 王俊博 于 2020-11-04 设计创作，主要内容包括：本发明涉及金属熔炼技术领域,具体涉及一种海绵锆的生产设备及工艺。本发明提供的一种海绵锆的生产设备,包括将升华炉和第一还原炉连接的通道,炉胆内置放熔化的液体镁,炉盖上设有镁的加料口、液镁的出口、测温压装置和供应惰性气的设备以及密闭连接的进气管,进气管上设有气泵和第二单向阀,在进气管下侧设有气爆管,进气管和第二单向阀之间设有气管支路,气管支路上设有第三单向阀和提供爆炸体的储物盒,爆炸体从气爆管的底部被惰性气的压力顶出并在炉胆内的镁液中爆炸加快了还原反应。本发明提高了海绵锆的生产效率和品质,取得了良好的经济效益和社会效益。(The invention relates to the technical field of metal smelting, in particular to a production device and a production process of sponge zirconium. The invention provides a production device of sponge zirconium, which comprises a passage for connecting a sublimation furnace and a first reduction furnace, wherein molten liquid magnesium is placed in a furnace liner, a magnesium feeding port, a liquid magnesium outlet, a temperature and pressure measuring device, an inert gas supplying device and a hermetically connected gas inlet pipe are arranged on a furnace cover, a gas pump and a second one-way valve are arranged on the gas inlet pipe, a gas explosion pipe is arranged on the lower side of the gas inlet pipe, a gas pipe branch is arranged between the gas inlet pipe and the second one-way valve, a third one-way valve and a storage box for providing an explosive body are arranged on the gas pipe branch, and the explosive body is ejected out from the bottom of the gas explosion pipe by the pressure of the inert gas and explodes in magnesium liquid in the furnace liner to accelerate reduction reaction. The invention improves the production efficiency and quality of the sponge zirconium and obtains good economic and social benefits.)

1. The production equipment of the sponge zirconium is characterized by comprising a sublimation furnace (30) and a first reduction furnace (10) which are communicated with each other through a channel (20) arranged at the top, wherein a first check valve (50) is arranged on the channel (20), a furnace liner (115) and a circulating water device (113) are arranged inside a furnace body (101) of the first reduction furnace (10), a heat preservation furnace material (103) is arranged between the furnace liner (115) and the furnace body (101), liquid magnesium which is heated and melted is arranged in the furnace liner (115), a temperature measuring port (102) for measuring the temperature and an electrical interface (114) for connecting with electrical equipment are arranged on the furnace body (101), the upper part of the furnace body (101) is hermetically connected with a furnace cover (106), a charging hole (110) for adding solid magnesium, an outlet (111) for the liquid magnesium, a temperature measuring device (112) and an air inlet pipe (107) hermetically connected with equipment for providing inert gas outside are respectively arranged on the furnace cover (106), an air pump (109) and a second one-way valve (108) are arranged at the upstream position of the air inlet pipe (107), an air explosion pipe (104) is arranged on the lower side of the air inlet pipe (107) in the furnace pipe (115), and an air outlet of the air explosion pipe (104) is arranged at the bottom of the magnesium liquid.

2. The production equipment of the sponge zirconium as claimed in claim 1, wherein a gas pipe branch is arranged between the inert gas inlet pipe (107) and the second one-way valve (108), a third one-way valve (117) and a storage box (116) for providing explosive bodies (118) are arranged on the gas pipe branch, a plurality of explosive bodies (118) are stored in the storage box (116), and the explosive bodies (118) are ejected from the bottom of the gas explosion pipe (104) by the pressure of the inert gas and are exploded in the magnesium liquid in the furnace pipe (115) to promote the reduction reaction.

3. The apparatus for producing zirconium sponge according to claim 2, wherein the explosive body (118) is a spherical structure, a spherical shell (119) is arranged outside the explosive body (118), and a core material ball (120) made of explosive material is arranged inside the explosive body (118).

4. The apparatus for producing zirconium sponge according to claim 3, wherein the shell (119) is made of graphite material.

5. The apparatus for producing zirconium sponge according to claim 3, wherein the shell (119) is made of a mixture of graphite and calcium carbonate.

6. The production equipment of zirconium sponge according to claim 5, wherein the mass ratio of the mixture of graphite and calcium carbonate is 1-2: 1.

7. the apparatus for producing zirconium sponge according to claim 6, wherein the mass ratio of the mixture of graphite and calcium carbonate is 1: 1. 1.5: 1 or 2: 1.

8. a process for manufacturing zirconium sponge according to any one of claims 1 to 7, characterized in that it comprises the following steps:

step 1, removing impurities in crude zirconium tetrachloride, namely putting the crude zirconium tetrachloride into a sublimation furnace (30), heating the sublimation furnace (30) to 331 ℃ for sublimation, and purifying the zirconium tetrachloride in the sublimation furnace (30) after the zirconium tetrachloride is changed into a gaseous state;

step 2, adding solid magnesium into a furnace pipe (115) from a feeding port (110) on the reduction furnace (10), opening switches of the reduction furnace (10) and a circulating water device (113) by using a control device, and heating the solid magnesium to 649-651 degrees to change metal magnesium into liquid magnesium;

step 3, opening a first one-way valve (50) on the channel (20), and conveying the purified gaseous zirconium tetrachloride in the sublimation furnace (30) into the reduction furnace (10);

and 4, opening switches of an air pump (109) and a second one-way valve (108), conveying inert gas to an air explosion pipe (104) through an air inlet pipe (107), allowing the inert gas to enter the bottom of the furnace pipe (115) from the air explosion pipe (104) and blow liquid magnesium, blowing the liquid magnesium at the bottom of the furnace pipe (115) upwards by inert gas airflow, blowing the liquid magnesium in the furnace pipe (115) upwards by airflow to form up-down flowing and regular circulating convection, turning the magnesium liquid up and down, and carrying out ZrCl on gaseous zirconium tetrachloride and the liquid magnesium which is continuously turned over in the reduction furnace (10)₄+2Mg＝2MgCl₂+ Zr reduction reaction;

step 5, opening a valve connected with the outlet (111) on the collecting device, and collecting the reduced sponge zirconium;

and 6, cooling the collected sponge zirconium to normal temperature, and storing the sponge zirconium at the normal temperature in a dry place.

9. The process for using the equipment for producing zirconium sponge as claimed in claim 8, wherein the process step 4 further comprises the following steps:

using a control device, closing the second one-way valve (108), opening the third one-way valve (117), pressing at least one explosive body (118) in the storage box (116) to the gas explosion tube (104) from a branch by using a high-pressure inert gas through the air pump (109), quickly pressing the explosive body (118) out of the gas explosion tube (104) by using the high-pressure gas, introducing the explosive body (118) into liquid magnesium at the bottom of the furnace container (115), exploding the explosive body (118) in the high-temperature magnesium liquid, enabling the magnesium liquid in the furnace container (115) to form irregular churning, and carrying out ZrCl on gaseous zirconium tetrachloride and the liquid magnesium in the reduction furnace (10)₄+2Mg＝2MgCl₂+ Zr takes place violent reduction reaction, produce sponge zirconium;

and then using the control device, closing the third one-way valve (117), opening the second one-way valve (108), conveying inert gas to the gas explosion pipe (104) through the gas inlet pipe (107), allowing the inert gas to enter the bottom of the furnace pipe (115) from the gas explosion pipe (104) to blow liquid magnesium again, blowing the liquid magnesium at the bottom of the furnace pipe (115) upwards by inert gas airflow, blowing the liquid magnesium in the furnace pipe (115) upwards by the airflow to form up-down regular circulating convection, enabling the magnesium liquid to form an up-down regular overturning state, and carrying out ZrCl on gaseous zirconium tetrachloride and the liquid magnesium which is continuously overturned in the reduction furnace (10)₄+2Mg＝2MgCl₂+ Zr reduction reaction;

the steps are alternately carried out, and the cyclic convection with regular and irregular alternation is formed.

10. The process for using the equipment for producing zirconium sponge as claimed in claim 9, wherein the explosive body (118) is pressed out from the gas explosion tube (104) and explodes in the liquid magnesium at the bottom of the furnace pipe (115), and the explosion occurs in the continuous explosion with the same time interval, and the frequency of the circulation convection which forms regular and irregular alternation is 1-3 times/10 minutes.

Technical Field

The invention belongs to the technical field of metal smelting, and particularly relates to production equipment and a production process of sponge zirconium.

Background

The sponge zirconium is also called as metal zirconium, is silver gray metal, has the appearance similar to steel, luster, very strong corrosion resistance and ultrahigh hardness and strength, and is mainly used for the aspects of aerospace, military industry, nuclear reaction and the like. Currently, the production of zirconium sponge mainly comprises two steps: the first step is to purify zirconium tetrachloride, remove impurities in crude zirconium tetrachloride and purify the zirconium tetrachloride; the second step is to adopt a Kroll method, and the production of the sponge zirconium is to carry out reduction reaction, namely, the zirconium tetrachloride after reduction and purification is reacted with magnesium to produce the sponge zirconium. In the process, zirconium tetrachloride can contact air, and can generate deliquescence to consume part of the zirconium tetrachloride, and the deliquescence can generate waste of the zirconium tetrachloride; in addition, there are also disadvantages that the reduction reaction efficiency of zirconium sponge is low and the reduction reaction efficiency is poor. In the production, zirconium tetrachloride and magnesium are respectively placed in a zirconium tetrachloride reaction furnace and a reduction furnace, the purified zirconium tetrachloride is in a gaseous state, metal magnesium in the reduction furnace is in a liquid state, the reduction furnace and the reduction furnace are connected through a passage, and the gaseous zirconium tetrachloride enters the reduction furnace filled with liquid magnesium to carry out reduction reaction to prepare the sponge zirconium, but the efficiency is low, and the quality of the produced sponge is low.

Disclosure of Invention

In order to solve the technical problems, the invention provides a production device and a production process of sponge zirconium, wherein the production device of sponge zirconium is provided with a gas explosion tube structure of inert gas and a process for gas explosion in magnesium liquid of a furnace liner and leading an explosive body to explode to increase the reduction efficiency, thereby achieving the purposes of improving the reduction reaction efficiency of sponge zirconium and improving the quality of sponge zirconium.

In order to achieve the purpose, the invention provides a production device of sponge zirconium, which comprises a sublimation furnace and a first reduction furnace which are communicated with each other through a channel arranged at the top, wherein a first one-way valve is arranged on the channel, a furnace liner and a circulating water device are arranged inside a furnace body of the first reduction furnace, heat-preservation furnace burden is arranged between the furnace liner and the furnace body, molten liquid magnesium is placed in the furnace liner, a temperature measuring port for measuring temperature and an electrical interface for connecting with electrical equipment are arranged on the furnace body, the upper part of the furnace body is hermetically connected with a furnace cover, a charging port for adding solid magnesium, an outlet for liquid magnesium, a temperature measuring and pressure device and a sealed air inlet pipe which is connected with equipment for providing inert gas outside are respectively arranged on the furnace cover, an air pump and a second one-way valve are arranged at the upstream position of the air inlet pipe, and an air explosion pipe is arranged at the lower side in the furnace, and the gas outlet of the gas explosion tube is arranged at the bottom of the magnesium liquid.

According to the preferable technical scheme, an air pipe branch is arranged between the air inlet pipe and the second one-way valve, a third one-way valve and a storage box for providing explosive bodies are arranged on the air pipe branch, a plurality of explosive bodies are stored in the storage box, and the explosive bodies are ejected out from the bottom of the gas explosion pipe by the pressure of inert gas and explode in magnesium liquid in the furnace pipe to promote reduction reaction.

According to the preferable technical scheme, the explosive body is of a spherical structure, a spherical shell is arranged outside the explosive body, and a core material ball made of explosive materials is arranged inside the explosive body.

According to the preferable technical scheme, the shell is made of graphite materials.

According to the preferable technical scheme, the shell is made of a mixture of graphite and calcium carbonate.

According to the preferable technical scheme, the mass ratio of the mixture of the graphite and the calcium carbonate is 1-2: 1.

according to the preferable technical scheme, the mass ratio of the mixture of the graphite and the calcium carbonate is 1: 1. 1.5: 1 or 2: 1.

the invention also provides a process for producing the zirconium sponge by using the equipment, which is characterized by comprising the following steps:

step 1, removing impurities in crude zirconium tetrachloride, namely putting the crude zirconium tetrachloride into a sublimation furnace, raising the temperature of the sublimation furnace to 331 ℃ for sublimation, and changing the zirconium tetrachloride in the sublimation furnace into a gaseous state for purification;

step 2, adding solid magnesium into the furnace pipe from a feed inlet on the reduction furnace, using a control device, opening switches of the reduction furnace and a circulating water device, and heating the solid magnesium to 649-651 ℃ to change metal magnesium into liquid magnesium;

step 3, opening a first one-way valve on the channel, and conveying the purified gaseous zirconium tetrachloride into a reduction furnace;

step 4, opening switches of the air pump and the second one-way valve, conveying inert gas to the gas explosion tube through the air inlet tube, allowing the inert gas to enter the bottom of the furnace pipe from the gas explosion tube and blowing liquid magnesium,the liquid magnesium at the bottom of the furnace is blown upwards by the inert gas flow, the liquid magnesium in the furnace is blown up by the gas flow to form the up-and-down flowing and regular circulating convection, so that the magnesium liquid is turned over up and down, and the gaseous zirconium tetrachloride and the liquid magnesium which is continuously turned over are subjected to ZrCl in the reduction furnace₄+2Mg＝2MgCl₂+ Zr reduction reaction;

step 5, opening a valve on a collecting device connected with the outlet, and collecting the reduced sponge zirconium;

and 6, cooling the collected zirconium sponge to normal temperature, and storing the normal-temperature zirconium sponge in a dry place.

In a preferred technical scheme, the process step 4 further comprises the following steps:

using a control device, closing the second one-way valve, opening the third one-way valve, pressing the explosive in the storage box to the gas explosion tube from the branch by the air pump by using high-pressure inert gas, rapidly pressing the explosive out of the gas explosion tube by the high-pressure gas, introducing the explosive into the liquid magnesium at the bottom of the furnace pipe, exploding the explosive in the high-temperature magnesium liquid to enable the magnesium liquid in the furnace pipe to form an irregular overturning state, and carrying out ZrCl reaction on gaseous zirconium tetrachloride and the liquid magnesium in the reduction furnace₄+2Mg＝2MgCl₂+ Zr takes place violent reduction reaction, produce sponge zirconium;

and then using the control device, closing the third one-way valve, opening the second one-way valve, conveying inert gas to the gas explosion pipe through the gas inlet pipe, blowing the liquid magnesium again by the inert gas flow entering the bottom of the furnace pipe from the gas explosion pipe, blowing the liquid magnesium at the bottom of the furnace pipe upwards by the inert gas flow, blowing the liquid magnesium in the furnace pipe again by the air flow, forming the circulation convection which is mutually regular up and down, enabling the magnesium liquid to form a vertically regular overturning state, and carrying out ZrCl on the gaseous zirconium tetrachloride and the liquid magnesium which is continuously overturned in the reduction furnace₄+2Mg＝2MgCl₂+ Zr reduction reaction;

the steps are alternately carried out, and the cyclic convection with regular and irregular alternation is formed.

According to the preferable technical scheme, the explosive body is pressed out from the gas explosion tube and enters the liquid magnesium at the bottom of the furnace pipe to explode, the time intervals of the explosion are the same, continuous explosion is realized, and the frequency control range of the regular and irregular alternate circulation convection is 1-3 times/10 minutes.

Compared with the prior art, the invention has the following beneficial effects:

1. the invention improves the reduction reaction efficiency in the production of the sponge zirconium, improves the quality of the sponge zirconium and also improves the economic benefit and the social benefit of energy conservation and environmental protection.

2. The invention solves the problems that in the production of sponge zirconium, zirconium tetrachloride is deliquesced and part of the zirconium tetrachloride is consumed.

Drawings

FIG. 1 is a plan view of an embodiment 1 of a production apparatus for zirconium sponge according to the present invention;

FIG. 2 is a left side view of FIG. 1;

fig. 3 is a sectional view of an inner structure of the first reduction furnace of fig. 1;

FIG. 4 is a structural view of a sublimation furnace in the invention;

FIG. 5 is another structural view of a sublimation furnace of the invention

FIG. 6 is another sectional view of the first reducing furnace in embodiment 2 of FIG. 1;

fig. 7 is a sectional view of the internal structure of the explosive body of fig. 6;

FIG. 8 is a top view of embodiment 3 of the present invention;

fig. 9 is a front view of embodiment 3 of the present invention.

Reference numerals

In the figure, 10-a first reduction furnace, 101-a furnace body, 102-a temperature measuring port, 103-a heat insulating furnace charge, 104-an air explosion tube, 105-a temperature resistant pad, 106-a furnace cover, 107-an air inlet tube, 108-a second one-way valve, 109-an air pump, 110-a charging port, 111-an outlet, 112-a temperature measuring device, 113-a circulating water device, 114-an electrical interface, 115-a furnace bladder, 116-a storage box, 117-a third one-way valve, 118-an explosive body, 119-a shell and 120-a core material ball; 20-a channel; 30-a sublimation furnace; 40-a second reduction furnace; 50-first check valve, 60-condensing furnace.

Detailed Description

Hereinafter, specific embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Example 1

As shown in fig. 1-2, the present embodiment provides a production apparatus of zirconium sponge, which includes a sublimation furnace 30 and a first reduction furnace 10, the sublimation furnace 30 and the first reduction furnace 10 are provided with a channel 20 at the top, the channel 20 arranged at the top connects the sublimation furnace 30 and the first reduction furnace 10, in order to adjust and control the amount of gaseous zirconium tetrachloride at any time, a first check valve 50 is provided on the channel 20, the sublimation furnace 30 can heat and purify zirconium tetrachloride therein, the purified zirconium tetrachloride is in a gaseous state, and magnesium metal in the first reduction furnace 10 is heated to a liquid state. As shown in fig. 3 and 4, the zirconium tetrachloride is purified in the sublimation furnace 30, in one way, a condensation furnace 60 is provided above the sublimation furnace 30, and the crude zirconium tetrachloride is purified to high-purity zirconium tetrachloride; another way is to purify the crude zirconium tetrachloride to high purity zirconium tetrachloride by passing hydrogen gas through the sublimation furnace 30. In this embodiment, the first reduction furnace 10 is a reduction furnace having a size of 400kg, the sublimation furnace 30 is a reduction furnace having a size of 1200kg, and 1200kg of zirconium tetrachloride purified by gasification is added to the first reduction furnace 10 containing 400kg of liquid magnesium through the passage 20 to perform a reduction reaction.

As shown in fig. 5, the specific structure of the first reduction furnace 10 includes a furnace bladder 115 and a water circulating device 113 arranged inside a furnace body 101 of the first reduction furnace 10, a heat insulating furnace charge 103 is arranged between the furnace bladder 115 and the furnace body 101, liquid magnesium to be heated and melted is placed in the furnace bladder 115, the furnace body 101 is provided with a temperature measuring port 102 for measuring temperature and an electrical interface 114 for connecting with electrical equipment, the upper part of the furnace body 101 is hermetically connected with a furnace cover 106, the furnace cover 106 is respectively provided with a charging port 110 for adding solid magnesium, an outlet 111 for liquid magnesium, a temperature measuring and pressure device 112 and an air inlet pipe connected with equipment for providing inert gas outside, in order to prevent reduction reaction from being affected, in this embodiment, the inert gas can be argon or helium, the inert gas equipment is hermetically connected with the air inlet pipe 107, an air pump 109 and a second one-way valve 108 are arranged at the upstream position of the, the gas explosion tube 104 is arranged at the lower side of the gas inlet pipe 107 in the furnace pipe 115, the gas outlet of the gas explosion tube 104 is arranged at the bottom of the magnesium liquid, the switch of the gas pump 109 and the second one-way valve 108 is opened, the second one-way valve 108 only admits gas and can not return gas reversely, and argon passes through the gas inlet pipe107 is conveyed into the gas explosion pipe 104 by the pressure of the gas pump 109, argon enters the bottom of the furnace pipe 115 from the gas explosion pipe 104 and blows the liquid magnesium in the furnace pipe, the liquid magnesium at the bottom of the furnace pipe 115 is blown upwards by the airflow of the argon, the liquid magnesium in the furnace pipe 115 forms regular circulating convection of up-and-down flow by the airflow blown from the outlet of the gas explosion pipe 104, the magnesium liquid forms a regular overturning state, the contact area between the magnesium liquid and zirconium tetrachloride is increased, and the gaseous zirconium tetrachloride and the liquid magnesium perform ZrCl in the reduction furnace 10₄+2Mg＝2MgCl₂The reduction reaction of Zr plays a role in accelerating the reduction reaction speed, and simultaneously improves the quality of the sponge zirconium; in order to increase the gas explosion effect, the airflow of the blown argon is more powerful, the turnover area of the magnesium liquid is larger, and in a preferable structure, a dune tube structure is arranged at the position of the gas outlet of the gas explosion tube 104; because the magnesium liquid can be continuously stirred up in the furnace pipe 115, the contact frequency and the contact area of the magnesium liquid and the gaseous zirconium tetrachloride are continuously increased, the effect of improving the reduction reaction efficiency of the zirconium tetrachloride and the liquid magnesium is achieved, and the quality of the sponge zirconium is improved in the reduction reaction.

The invention provides an equipment production process of sponge zirconium, which comprises the following steps:

step 1, removing impurities in crude zirconium tetrachloride, namely putting the crude zirconium tetrachloride into a sublimation furnace 30, raising the temperature of the sublimation furnace 30 to 331 ℃ for sublimation, and changing the zirconium tetrachloride in the sublimation furnace 30 into a purified gas state;

step 2, adding solid magnesium into the furnace pipe 115 from a feeding hole 110 on the reduction furnace 10, using a control device, opening switches of the reduction furnace 10 and a water circulating device 113, controlling the heating temperature range of the solid magnesium to be 649-651 degrees, and changing the solid magnesium metal into liquid magnesium;

step 3, opening a first one-way valve 50 on the channel 20, and conveying the purified gaseous zirconium tetrachloride into the reduction furnace 10;

step 4, opening switches of the air pump 109 and the second one-way valve 108, conveying argon gas to the gas explosion tube 104 through the air inlet pipe 107, allowing the argon gas to enter the bottom of the furnace pipe 115 from the gas explosion tube 104 and blow liquid magnesium, and allowing the liquid magnesium at the bottom of the furnace pipe 115 to be blown upwards by the flow of the argon gasBlowing out the gas flow to form circulating convection of the liquid magnesium in the furnace pipe 115 flowing up and down to make the magnesium liquid turn over, and the gaseous zirconium tetrachloride and the liquid magnesium perform ZrCl reaction in the reduction furnace 10₄+2Mg＝2MgCl₂+ Zr reduction reaction;

step 5, opening a valve on a collecting device connected with the outlet 111, and collecting the reduced sponge zirconium;

and 6, cooling the collected zirconium sponge to normal temperature, and storing the normal-temperature zirconium sponge in a dry place.

Example 2

This example is further improved on the basis of example 1, with the difference that: as shown in fig. 6, in the production apparatus of zirconium sponge provided in this embodiment, an air pipe branch is provided between the air inlet pipe 107 and the second check valve 108, a third check valve 117 and a storage box 116 for providing explosive 118 are provided on the air pipe branch, a plurality of explosive 118 are stored in the storage box 116, the air pump 109 first uses negative pressure to suck the explosive 118 into the branch, and then uses generated positive pressure to press the explosive 118 into the air inlet pipe 107 and the air explosion pipe 104, and the explosive 118 is ejected from the bottom of the air explosion pipe 104 by the pressure of argon gas and explodes in the magnesium liquid in the furnace bladder 115. In this embodiment, as shown in fig. 7, the explosive 118 is configured to be a spherical structure, the outer portion of the explosive 118 is a spherical shell 119, the inner portion of the explosive 118 is a core ball 120 made of an explosive material, because ammonium nitrate has the characteristic of exploding when heated, the core ball 120 is made of an ammonium nitrate material, the mass of the core ball 120 made of ammonium nitrate is selected to be 1-8 g, the selection is performed according to the depth of the gas explosion tube 104 extending into the liquid magnesium in the furnace pipe 115, and the deeper the extending depth is, the larger the mass of the selected core ball 120 is, and the core ball 120 with a mass of 1 g, 3 g, 5 g or 8 g is preferred; because graphite has stable chemical properties and can react with oxygen and other impurities to remove impurities, the shell 119 is preferably made of graphite material; wherein, the technical proposal is further optimized, the shell 119 is made of a mixture of graphite and calcium carbonate, wherein the calcium carbonate; according to the preferable technical scheme, the mass ratio of the mixture of the graphite and the calcium carbonate is 1-2: 1, the mass ratio of the graphite to the calcium carbonate mixture is preferably 1: 1. 1.5: 1 or 2: 1; in this example, the mass ratio of the mixture of graphite and calcium carbonate was 1.5: 1.

the invention also provides a production process using the equipment for producing the sponge zirconium, and in the process step 4 in the embodiment 1, the production process further comprises the following steps:

using a control device, firstly closing the second one-way valve 108, opening the third one-way valve 117, pressing at least one explosive 118 in the storage box 116 to the gas explosion tube 104 from a branch by the high-pressure inert gas through the air pump 109, rapidly pressing the explosive 118 out of the gas explosion tube 104 by the high-pressure gas, and allowing the explosive 118 to enter liquid magnesium at the bottom of the furnace pipe 115, wherein the explosive 118 explodes in high-temperature magnesium liquid, so that the magnesium liquid in the furnace pipe 115 forms an irregular overturning state, and gaseous zirconium tetrachloride and the liquid magnesium perform ZrCl in the reduction furnace 10₄+2Mg＝2MgCl₂+ Zr takes place violent reduction reaction, produce the sponge zirconium of high quality, has raised the production efficiency of producing sponge zirconium;

then, the control device is used, the third one-way valve 117 is closed, the second one-way valve 108 is opened, the inert gas is conveyed to the gas explosion tube 104 through the gas inlet pipe 107, the argon enters the bottom of the furnace pipe 115 from the gas explosion tube 104 and blows the liquid magnesium, the liquid magnesium at the bottom of the furnace pipe 115 is blown upwards by the argon gas flow, the liquid magnesium in the furnace pipe 115 is blown up by the air flow to form the circulation convection with the relative regular upper and lower phases, the magnesium liquid is enabled to form the regular upper and lower overturning state, and the gaseous zirconium tetrachloride and the liquid magnesium which is continuously overturned are subjected to ZrCl in the reduction furnace 10₄+2Mg＝2MgCl₂+ Zr reduction reaction;

the steps are alternately carried out to form regular and irregular alternate circulation convection;

in this embodiment, the shell 119 is made of graphite material, in which the graphite mainly contains carbon, and the carbon can react with impurities in zirconium tetrachloride, for example, oxygen in the graphite can react to produce carbon monoxide or carbon dioxide, and oxygen in the zirconium tetrachloride can be removed, so that the produced zirconium sponge has higher quality; according to the preferred technical scheme, the shell 119 is made of a mixture of graphite and calcium carbonate, wherein the calcium carbonate can react with impurities in zirconium tetrachloride to generate slag, and the slag floats on the surface of liquid magnesium in the reduction furnace 10 to adsorb the impurities, so that the quality of the sponge zirconium is improved; in addition, calcium carbonate can react with chlorine in zirconium tetrachloride to generate calcium chloride and zirconium, and the efficiency of reduction reaction is increased.

In this embodiment, since the explosive 118 is pressed out from the gas explosion tube 104 into the liquid magnesium at the bottom of the furnace pipe 115 to explode, the preferred technical scheme is to set the explosion time and interval to be the same continuous explosion, i.e. the frequency of forming the regular and irregular alternate circulation convection is 1-3 times/10 minutes.

Example 3

On the basis of embodiments 1 and 2, the present embodiment is further improved, with the difference that: as shown in fig. 8 and 9, a first reduction furnace 10 and a second reduction furnace 40 are connected to a sublimation furnace 30 through a passage 20, the first reduction furnace 10 and the second reduction furnace 40 have the same structure, which doubles the production energy, and if 2400kg of zirconium tetrachloride is consumed, two reduction furnaces for reacting 1200kg of zirconium tetrachloride with 400kg of magnesium are required to co-deliquesce about 200kg of zirconium tetrachloride, and the sublimation furnace containing 2400kg of zirconium tetrachloride is connected to two reduction furnaces for containing 400kg of liquid magnesium, deliquescence is reduced to 100kg, which plays a role in saving raw materials as it is wasted by consuming 1200kg of zirconium tetrachloride; for single consumption 1200kg zirconium tetrachloride the number of times that has reduced the air that exposes in the dismouting pipeline in-process, improved the purity that generates the zirconium sponge, owing to adopt 1 sublimation stove 30 to 2 reduction furnaces 10's mode, embodied the effect of the current factory building space of make full use of, when originally consuming 1200kg zirconium tetrachloride, directly consume 2400kg zirconium tetrachloride, reached and reduced the cost of labor, save time and the purpose of raising the efficiency.

The preferred embodiments and examples have been described in detail with reference to the accompanying drawings, but the invention is not limited to the embodiments and examples described above, and various changes can be made within the knowledge of those skilled in the art without departing from the present concept.