Liquid magnesium purification device and purification method for titanium sponge production

Abstract

The invention belongs to the technical field of liquid magnesium purification, and particularly relates to a liquid magnesium purification device and purification method for titanium sponge production. The liquid magnesium purification device is reasonable in design, the crucible large cover and the crucible device are detachably and hermetically connected, sediment cleaning and repeated use are facilitated, and liquid magnesium to be purified is effectively purified by arranging the magnesium outlet, the pressurizing opening, the pressure relief opening and the feeding opening. The feeding device is provided with a flow meter, a regulating valve and other components, the adding amount of a purification material can be accurately controlled, and the stability and consistency of the purification effect are ensured. The purification material reacts with the liquid magnesium at high temperature to generate sponge titanium, impurity components in the liquid magnesium are adsorbed through the adsorption effect of the sponge titanium, and meanwhile generated magnesium chloride precipitates at the bottom of the crucible due to the fact that the density of the generated magnesium chloride is larger than that of the liquid magnesium, so that the problem that impurities cannot be effectively reduced due to standing sedimentation of an existing crucible is solved; and the quality of the produced sponge titanium is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of liquid magnesium purification, and in particular relates to a liquid magnesium purification device and a purification method for sponge titanium production. Background Art

[0002] In order to reduce the excessive amount of impurities such as iron and aluminum in liquid magnesium entering into sponge titanium, a crucible is usually left to stand for impurity sedimentation to achieve the purpose of purifying the liquid magnesium; however, sedimentation cannot effectively reduce the impurities in the liquid magnesium. Therefore, when liquid magnesium needs to be added for the production of sponge titanium, all the impurities in the added liquid magnesium enter the sponge titanium. Due to the adsorption characteristics of sponge titanium, the impurities in the liquid magnesium are enriched in the sponge titanium, causing the quality of the sponge titanium to deteriorate, which in turn affects the market price of sponge titanium and causes certain economic losses to the company.

[0003] Therefore, there is an urgent need for a liquid magnesium purification device to solve the problem that the prior art cannot effectively reduce impurities in the liquid magnesium. Summary of the invention

[0004] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a liquid magnesium purification device and a purification method for sponge titanium production.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] On the one hand, the present invention provides a liquid magnesium purification device for sponge titanium production, comprising a crucible device for heating and keeping the liquid magnesium warm, and a large crucible cover detachably and hermetically connected to the crucible device;

[0007] The top surface of the crucible cover is provided with a magnesium outlet, a pressure charging port for charging inert gas, a pressure relief port for discharging inert gas, and a feeding port for adding purified material; the magnesium outlet is provided with a second flange connected to a sealing cover, the pressure relief port is provided with a pluggable sealing plug, and the feeding port is connected to a feeding device for conveying purified material.

[0008] Specifically, the crucible device includes a crucible and a heating device wrapped outside the crucible and used for heating and heat preservation.

[0009] Specifically, the crucible cover is also provided with a first flange sealedly connected to the crucible device.

[0010] Furthermore, a sealing rubber ring is provided between the first flange and the crucible device.

[0011] Specifically, a pressure measuring port is provided on the top surface of the large crucible cover, and a pressure measuring device for detecting the pressure of the inert gas in the crucible device is fixedly provided on the pressure measuring port.

[0012] Specifically, the charging port is connected to an inert gas storage tank, and a first valve is provided between the inert gas storage tank and the charging port.

[0013] Specifically, the feeding device includes a purification material storage tank, the feeding device is provided with a hollow feeding rod for inserting into the feeding port, the hollow feeding rod is sealed and connected to the feeding port, a second valve is provided at one end of the hollow feeding rod away from the feeding port, a third valve, a flow meter, and a regulating valve are provided in sequence between the purification material storage tank and the second valve, and a fourth valve for pressure relief is provided between the second valve and the regulating valve; preferably, the hollow feeding rod extends into the lower middle part of the crucible to pass the purification material.

[0014] Specifically, the purification material is titanium tetrachloride.

[0015] Specifically, the sealing plug is sealed with the pressure relief port, and the sealing plug is made of rubber.

[0016] It should be noted that titanium tetrachloride reacts with magnesium at high temperature to produce titanium sponge. The main chemical reaction formula is as follows:

[0017]

[0018] The adsorption effect of the generated titanium sponge is utilized to adsorb the impurity components in the liquid magnesium, and the density of the generated magnesium chloride is greater than the density of the liquid magnesium, so the magnesium chloride and the liquid magnesium are separated and precipitated at the bottom of the crucible.

[0019] On the other hand, the present invention provides a purification method for a liquid magnesium purification device for sponge titanium production, the specific steps of which are as follows:

[0020] Step 1, first add the liquid magnesium to be purified into the crucible device, and then seal and connect the crucible cover to the crucible device;

[0021] Step 2, heating the crucible device to 790-800°C and keeping the temperature constant;

[0022] Step 3, charging the pressure port with an inert gas at a preset pressure of 3-5 kPa;

[0023] Step 4: using a feeding device to add a specific amount of a hollow rod of a purification material into the liquid magnesium to be purified, and letting it stand for a preset time; the preset standing time is greater than or equal to 2 hours;

[0024] Step 5, pull out the sealing plug to discharge the inert gas;

[0025] Step 6: Open the magnesium outlet and extract the purified liquid magnesium to obtain liquid magnesium for sponge titanium production.

[0026] Specifically, in step 4, the specific function of standing is to allow the magnesium chloride generated by the reaction to precipitate to the bottom of the crucible and to allow the titanium sponge to have sufficient time to absorb impurities, thereby making the liquid magnesium purer.

[0027] It should be noted that in actual production, after the crucible cover is sealed and connected to the crucible device, the liquid magnesium to be purified is purified and used for titanium production after purification; when the liquid magnesium needs to be further purified subsequently, the liquid magnesium to be purified needs to be added to the liquid magnesium purification device from the magnesium outlet; in addition, when the liquid magnesium purification device is in use, the crucible device continues to keep warm until the precipitate in the crucible device needs to be cleaned, then the heating device is turned off, the crucible cover is opened, and after the precipitate in the crucible device is cleaned, the above steps are repeated to purify the liquid magnesium to be purified.

[0028] In addition, after the liquid magnesium to be purified in the liquid magnesium purification device reacts with the purification material, it can be left to stand for 2 hours, and then the purified liquid magnesium can be extracted, or it can be left to stand for more than 2 hours before extracting the purified liquid magnesium according to actual production needs; when it is necessary to extract the purified liquid magnesium, the pipeline for extracting the liquid magnesium needs to be extended into the liquid magnesium, preferably half the height of the liquid magnesium; if it is extended too deep, the precipitate will easily be extracted together, affecting its use.

[0029] In addition, after the purified liquid magnesium is extracted, it is supplemented with liquid magnesium to be purified and purification is continued. Each time the liquid magnesium to be purified is added, it is necessary to charge the matching purification material, that is, 1 t of liquid magnesium to be purified needs to be fed with 4.2 kg of purification material.

[0030] Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects:

[0031] 1. The liquid magnesium purification device of the present invention is reasonably designed. The crucible cover and the crucible device are detachable and sealed, which is convenient for cleaning precipitation and reuse. The liquid magnesium to be purified is effectively purified by arranging a magnesium outlet, a pressure charging port, a pressure relief port and a feeding port.

[0032] 2. The present invention provides a flow meter, a regulating valve and other components through the feeding device, which can accurately control the amount of purification material added. For example, 4.2 kg of purification material is introduced into 1 t of liquid magnesium to be purified, thereby ensuring the stability and consistency of the purification effect.

[0033] 3. The present invention generates sponge titanium by reacting purified materials with liquid magnesium at high temperature, and utilizes the adsorption effect of sponge titanium to adsorb impurities in the liquid magnesium. Meanwhile, the generated magnesium chloride is precipitated at the bottom of the crucible because of its density greater than that of the liquid magnesium. This solves the problem that the existing crucible cannot effectively reduce impurities by static sedimentation, and improves the quality of sponge titanium production. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The accompanying drawings are incorporated in and constitute a part of this specification and, together with the description, serve to explain the principles of the present invention.

[0035] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0036] Figure 1 This is a schematic structural diagram of a liquid magnesium purification device for titanium sponge production according to the present invention;

[0037] Figure 2 A top view of the crucible cover of the present invention;

[0038] Figure 3 for Figure 2 AA section view;

[0039] Figure 4 It is a schematic diagram of the structure of the feeding device of the present invention;

[0040] Figure 5 Flow chart of the purification method of the present invention.

[0041] Among them: 1 is the magnesium outlet; 2 is the pressure charging port; 3 is the pressure measuring port; 4 is the pressure relief port; 5 is the feeding port; 6 is the sealing plug; 7 is the crucible cover; 8 is the crucible; 9 is the heating device; 10 is the purification material storage tank; 11 is the third valve; 12 is the flow meter; 13 is the regulating valve; 14 is the second valve; 15 is the fourth valve; 16 is the hollow rod for passing materials. DETAILED DESCRIPTION

[0042] Here, exemplary embodiments will be described in detail, and examples thereof are shown in the accompanying drawings. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Instead, they are only examples consistent with some aspects of the present invention as detailed in the appended claims.

[0043] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments.

[0044] See also Figure 1-4 As shown, the present invention provides a liquid magnesium purification device for sponge titanium production, comprising a crucible device for heating and keeping the liquid magnesium warm, and a large crucible cover 7 detachably and hermetically connected to the crucible device;

[0045] The top surface of the crucible cover 7 is provided with a magnesium outlet 1, a pressure charging port 2 for charging inert gas, a pressure relief port 4 for discharging inert gas, and a feeding port 5 for adding purified material; the magnesium outlet 1 is provided with a second flange connected to a sealing cover, the pressure relief port 4 is provided with a pluggable sealing plug 6, and the feeding port 5 is connected to a feeding device for conveying purified material.

[0046] Specifically, the crucible device includes a crucible 8 and a heating device 9 wrapped outside the crucible 8 and used for heating and heat preservation, see Figure 1 shown.

[0047] Specifically, the crucible cover 7 is also provided with a first flange sealedly connected to the crucible device.

[0048] Furthermore, a sealing rubber ring is provided between the first flange and the crucible device.

[0049] Specifically, a pressure measuring port 3 is further provided on the top surface of the crucible cover 7, and a pressure measuring device for detecting the pressure of the inert gas in the crucible device is fixedly provided on the pressure measuring port 3.

[0050] Specifically, the charging port 2 is connected to an inert gas storage tank, and a first valve is provided between the inert gas storage tank and the charging port 2 .

[0051] Specifically, the feeding device includes a purification material storage tank 10, the feeding device is provided with a hollow rod 16 for inserting into the feeding port 5, the hollow rod 16 is sealed and connected to the feeding port 5, a second valve 14 is provided at one end of the hollow rod 16 away from the feeding port 5, a third valve 11, a flow meter 12, and a regulating valve 13 are provided between the purification material storage tank 10 and the second valve 14 in sequence, and a fourth valve 15 for pressure relief is provided between the second valve 14 and the regulating valve 13; preferably, the hollow rod is extended into the middle and lower part of the crucible to pass the purification material, see Figure 4 shown.

[0052] Specifically, the purification material is titanium tetrachloride.

[0053] Specifically, the sealing plug 6 is in sealing cooperation with the pressure relief port 4 , and the sealing plug 6 is made of rubber.

[0054] Example 1

[0055] See also Figure 5 As shown, this embodiment also provides a purification method for a liquid magnesium purification device for sponge titanium production, and the specific steps are as follows:

[0056] Step 1, first add 2t of liquid magnesium to be purified into the crucible device, and then seal the crucible cover 7 with the crucible device;

[0057] Step 2, heating the crucible device to 790° C. and keeping the temperature constant;

[0058] Step 3, filling 3 kPa of inert gas into the pressure charging port 2;

[0059] Step 4: Use a feeding device to add 8.4 kg of the purified material hollow rod into the liquid magnesium to be purified, and let it stand for 2 hours;

[0060] Step 5, pull out the sealing plug 6 to discharge the inert gas;

[0061] Step 6: Open the magnesium outlet 1 to extract the purified liquid magnesium in the crucible device to obtain liquid magnesium for sponge titanium production.

[0062] Example 2

[0063] See also Figure 5 As shown, this embodiment also provides a purification method for a liquid magnesium purification device for sponge titanium production, and the specific steps are as follows:

[0064] Step 1, first add 4t of liquid magnesium to be purified into the crucible device, and then seal the crucible cover 7 with the crucible device;

[0065] Step 2, heating the crucible device to 800° C. and keeping the temperature constant;

[0066] Step 3, filling 5 kPa of inert gas into the pressure charging port 2;

[0067] Step 4: Use a feeding device to add 16.8 kg of the purified material hollow rod into the liquid magnesium to be purified, and let it stand for 3 hours;

[0068] Step 5, pull out the sealing plug 6 to discharge the inert gas;

[0069] Step 6: Open the magnesium outlet 1 to extract the purified liquid magnesium in the crucible device to obtain liquid magnesium for sponge titanium production.

[0070] It should be noted that the adsorption time of the impurities in the generated sponge titanium and the liquid magnesium to be purified is 2 hours. However, in actual production, the liquid magnesium to be purified will not be extracted immediately after purification, but will be extracted when needed; therefore, the adsorption time of the impurities in the sponge titanium and the liquid magnesium to be purified is greater than or equal to 2 hours; when it is necessary to extract the liquid magnesium, first pull out the sealing plug 6, discharge the inert gas, and then perform the liquid magnesium extraction operation.

[0071] The above description is only a specific embodiment of the present invention, so that those skilled in the art can understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention.

[0072] It should be understood that the present invention is not limited to what has been described above and that various modifications and changes may be made without departing from its scope. The scope of the present invention is limited only by the appended claims.

Claims

1. A liquid magnesium purification device for titanium sponge production, characterized in that: It comprises a crucible device for heating and keeping liquid magnesium warm, and a large crucible cover (7) which is detachably and hermetically connected to the crucible device; The top surface of the crucible cover (7) is provided with a magnesium outlet (1), a pressure charging port (2) for charging inert gas, a pressure relief port (4) for discharging inert gas, and a feeding port (5) for adding purification material; the magnesium outlet (1) is provided with a second flange connected to a sealing cover, the pressure relief port (4) is provided with a pluggable sealing plug (6), and the feeding port (5) is connected to a feeding device for conveying purification material; the crucible device comprises a crucible (8) and a heating device (9) wrapped outside the crucible (8) and used for heating and heat preservation; the crucible cover (7) is also provided with a first flange sealed and connected to the crucible device.

2. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: A sealing rubber ring is provided between the first flange and the crucible device.

3. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The top surface of the crucible cover (7) is also provided with a pressure measuring port (3), and a pressure measuring device for detecting the pressure of the inert gas in the crucible device is fixedly provided on the pressure measuring port (3).

4. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The pressure charging port (2) is connected to an inert gas storage tank, and a first valve is provided between the inert gas storage tank and the pressure charging port (2).

5. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The feeding device comprises a purified material storage tank (10), the feeding device is provided with a hollow material passing rod (16) for inserting into a feeding port (5), the hollow material passing rod (16) is sealedly connected to the feeding port (5), a second valve (14) is provided at one end of the hollow material passing rod (16) away from the feeding port (5), a third valve (11), a flow meter (12), and a regulating valve (13) are provided in sequence between the purified material storage tank (10) and the second valve (14), and a fourth valve (15) for pressure relief is provided between the second valve (14) and the regulating valve (13).

6. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The purification material is titanium tetrachloride.

7. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The sealing plug (6) is in sealing cooperation with the pressure relief port (4).

8. The liquid magnesium purification device for titanium sponge production according to claim 1, characterized in that: The sealing plug (6) is made of rubber.

9. A purification method for a liquid magnesium purification device for titanium sponge production according to any one of claims 1 to 8, characterized in that: The specific steps are as follows: Step 1, first add the liquid magnesium to be purified into the crucible device, and then seal and connect the crucible cover (7) to the crucible device; Step 2, heating and keeping the crucible device warm; Step 3, charging the pressure charging port (2) with an inert gas at a preset pressure; Step 4: Add a specific amount of purification material to the feed port (5) and let it stand for a preset time; Step 5, pull out the sealing plug (6) to discharge the inert gas; Step 6: Open the magnesium outlet (1) to extract the purified liquid magnesium to obtain liquid magnesium for titanium sponge production.

10. The purification method of the liquid magnesium purification device for titanium sponge production according to claim 9, characterized in that: The heating temperature of the crucible device is 790-800°C.

Images