A distillation method for improving the volatilization efficiency of magnesium chloride

Abstract

This invention relates to the field of titanium metal smelting technology, specifically to a distillation method for improving the volatilization efficiency of magnesium chloride. The method includes: after reduction, assembling the distillation apparatus and placing it into a distillation furnace; after ensuring proper sealing, heating the distillation furnace, which is divided into four zones from top to bottom: Zones 1, 2, 3, and 4; in the first stage, heating zones 1 and 4 to a specified temperature and holding them there, ensuring zone 4 is 300°C higher than zone 1; in the second stage, heating zones 2 and 3 to a specified temperature and holding them there; in the third stage, turning off heating in zone 1 while maintaining the temperature in zones 2, 3, and 4 for a certain period and controlling the vacuum level; in the fourth stage, turning on heating in zone 1, adjusting zones 1, 2, 3, and 4 to a specified temperature, holding them there for a certain period, and then determining the endpoint; after distillation, transferring the equipment to a cooling station. This invention employs a staged distillation method, establishing a distillation route from both ends to the center; this effectively avoids sintering, ensuring maximum volatilization of magnesium chloride while preventing capillary sintering and the introduction of iron impurities caused by prolonged high temperatures.

Description

Technical Field

[0001] This invention relates to the field of titanium metal smelting technology, and more specifically, to a distillation method for improving the volatilization efficiency of magnesium chloride. Background Technology

[0002] Titanium sponge is widely used in aerospace, shipbuilding, metallurgy, chemical, automotive and energy fields due to its low density, high specific hardness, excellent high and low temperature resistance, and corrosion resistance. It is also an important raw material for the preparation of titanium materials and other titanium components. Currently, the commercial production method of titanium sponge at home and abroad is the magnesium thermal reduction of titanium tetrachloride. This method mainly includes three major processes: magnesium reduction of titanium tetrachloride, vacuum distillation of the reduction product, and crushing and processing of the product.

[0003] Reduction and distillation are the core processes in the production of sponge titanium and are crucial in determining the quality of the product. Taking vacuum distillation as an example, this step is directly influenced by chlorine. However, current distillation methods heat the entire furnace simultaneously, neglecting the issue of uneven heating between the top and bottom of the titanium mass and its center. Therefore, to address this issue, we propose a distillation method that improves the volatilization efficiency of magnesium chloride. Summary of the Invention

[0004] The purpose of this invention is to provide a distillation method that improves the volatilization efficiency of magnesium chloride, so as to solve the problems mentioned in the background art.

[0005] To solve the above-mentioned technical problems, the present invention aims to provide a distillation method for improving the volatilization efficiency of magnesium chloride, comprising the following steps:

[0006] S1. After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test.

[0007] S2. After the sealing test is qualified, the distillation furnace is heated. The distillation furnace is divided into zones 1, 2, 3 and 4 from top to bottom. In the first stage, the temperature of zones 1 and 4 is raised to the specified temperature and then kept at that temperature. Zone 4 is kept 300°C higher than zone 1 for a certain period of time. The heating rate in this stage is controlled at 5°C / min.

[0008] S3, the second stage, heating of zones 2 and 3 is started, heating zones 2 and 3 to the specified temperature and maintaining it for a certain time, and the heating rate during this stage is controlled at 5℃ / min;

[0009] S4. In the third stage, the heating in zone 1 is turned off, while zones 2, 3, and 4 continue to maintain the above temperature for a certain period of time, and the vacuum degree is controlled within the specified range.

[0010] S5. In the fourth stage, zone 1 heating is activated. The temperatures of zones 1, 2, 3, and 4 are adjusted to the specified temperatures and maintained for a certain period of time before the endpoint is determined.

[0011] S6. After distillation, transfer to the cooling station.

[0012] As a further improvement to this technical solution, in step S2, the temperature control range of zone 1 is 610-620℃, the temperature control range of zone 4 is 910-920℃, and the heat preservation time is controlled at 2-4h.

[0013] As a further improvement to this technical solution, in step S3, the temperature control range of zones 2 and 3 is 910-920℃, and the heat preservation time is controlled at 5-7h.

[0014] As a further improvement to this technical solution, in step S4, the temperature control range of zones 2, 3, and 4 is 910-920℃, the heat preservation time is controlled at 10-12h, and the vacuum degree control range is 10-15Pa.

[0015] As a further improvement to this technical solution, in step S5, the temperature control range of zones 1, 2, 3, and 4 is 1040-1050℃, and the heat preservation time is controlled at 50-70h.

[0016] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0017] 1. The distillation method for improving the volatilization efficiency of magnesium chloride adopts a staged distillation approach. Based on the different volatilization efficiencies of magnesium chloride inside and outside the titanium block, a specific scheme was formulated. The core is the most difficult to volatilize, so it is necessary to slowly heat up and preheat in the early stage, and control the heating time of the upper and lower parts separately, i.e., the distillation route from both ends to the center.

[0018] 2. This distillation method for improving the volatilization efficiency of magnesium chloride can effectively avoid sintering caused by directly heating to a high temperature. Different heating times are set for each zone according to different conditions, which can ensure that magnesium chloride is volatilized and removed as much as possible, and also prevent capillary sintering and the introduction of iron impurities caused by prolonged high temperature. Attached Figure Description

[0019] Figure 1 This is an exemplary overall method flowchart of the present invention. Detailed Implementation

[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0021] Example 1

[0022] like Figure 1 As shown, this embodiment provides a distillation method for improving the volatilization efficiency of magnesium chloride, including the following steps:

[0023] S1. After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test.

[0024] S2. After the sealing test is qualified, the distillation furnace is heated. The distillation furnace is divided into zones 1, 2, 3 and 4 from top to bottom. In the first stage, zone 1 is heated to 610℃ and zone 4 is heated to 910℃. Zone 4 is kept 300℃ higher than zone 1 and maintained for 2 hours. The heating rate is controlled at 5℃ / min.

[0025] S3, the second stage, zones 2 and 3 heating is turned on, the temperature is raised to 910℃ and maintained for 5 hours, the heating rate is controlled at 5℃ / min;

[0026] S4. In the third stage, turn off the heating in zone 1, and continue to maintain the above temperature in zones 2, 3 and 4 for 10 hours, while controlling the vacuum degree at 10Pa.

[0027] S5. In the fourth stage, start heating in zone 1, adjust the temperature of zones 1, 2, 3 and 4 to 1040℃, maintain it for 50 hours and then determine the endpoint.

[0028] S6. After distillation, transfer to the cooling station.

[0029] Example 2

[0030] This embodiment provides a distillation method to improve the volatilization efficiency of magnesium chloride, based on Example 1, including the following steps:

[0031] S1. After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test.

[0032] S2. After the sealing test is qualified, the distillation furnace is heated. The distillation furnace is divided into four zones from top to bottom: 1, 2, 3, and 4. In the first stage, the temperature of zone 1 is raised to 615℃ and the temperature of zone 4 is raised to 915℃. Zone 4 is kept 300℃ higher than zone 1 and maintained for 3 hours. The heating rate is controlled at 5℃ / min.

[0033] S3, the second stage, zones 2 and 3 heating is turned on, the temperature is raised to 915℃ and maintained for 6 hours, the heating rate is controlled at 5℃ / min;

[0034] S4. In the third stage, turn off the heating in zone 1, and continue to maintain the above temperature in zones 2, 3 and 4 for 11 hours, while controlling the vacuum degree at 13 Pa.

[0035] S5. In the fourth stage, start heating in zone 1, adjust the temperature of zones 1, 2, 3 and 4 to 1045℃, maintain it for 60 hours and then determine the endpoint.

[0036] S6. After distillation, transfer to the cooling station.

[0037] Example 3

[0038] This embodiment provides a distillation method to improve the volatilization efficiency of magnesium chloride, based on Example 1, including the following steps:

[0039] S1. After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test.

[0040] S2. After the sealing test is qualified, the distillation furnace is heated. The distillation furnace is divided into four zones from top to bottom: 1, 2, 3, and 4. In the first stage, the temperature of zone 1 is raised to 620℃ and the temperature of zone 4 is raised to 920℃. Zone 4 is kept 300℃ higher than zone 1 and maintained for 4 hours. The heating rate is controlled at 5℃ / min.

[0041] S3, the second stage, zones 2 and 3 heating is turned on, the temperature is raised to 920℃ and maintained for 7 hours, the heating rate is controlled at 5℃ / min;

[0042] S4. In the third stage, turn off the heating in zone 1, and continue to maintain the above temperature in zones 2, 3 and 4 for 12 hours, while controlling the vacuum degree at 15 Pa.

[0043] S5. In the fourth stage, start heating in zone 1, adjust the temperature of zones 1, 2, 3 and 4 to 1050℃, maintain this temperature for 70 hours and then determine the endpoint.

[0044] S6. After distillation, transfer to the cooling station.

[0045] Comparative Example

[0046] Based on currently common operating methods, this embodiment provides a conventional method for distilling sponge titanium, including the following steps:

[0047] Step 1: After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test.

[0048] Step 2: After the sealing test is passed, the distillation furnace is heated. The distillation furnace is divided into 1, 2, 3 and 4 zones from top to bottom. All zones are heated to 1050℃ and maintained for 80-100 hours to determine the endpoint. The vacuum degree is controlled at 10-15Pa.

[0049] Step 3: After distillation, transfer to the cooling station.

[0050] This embodiment also compares the effects of the sponge titanium distillation methods in Examples 1, 2, 3, and the comparative example through specific applications and experiments, as shown in the table below:

[0051] Example 1 0.045 88 Example 2 0.044 85 Example 3 0.045 90 Comparative Example 0.06 120

[0052] As can be seen from the table, regardless of whether the application schemes in Examples 1, 2, or 3 are used, the chloride (Cl) content in the distilled sponge titanium can be effectively reduced, thus improving the volatilization efficiency of magnesium chloride and effectively shortening the distillation time. In summary, the method of this invention can effectively improve the volatilization efficiency of magnesium chloride during the distillation of sponge titanium, shorten the distillation time, improve operational efficiency, and enhance the quality of the finished sponge titanium.

[0053] Those skilled in the art will understand that the process of implementing all or part of the steps of the above embodiments can be carried out by hardware or by a program instructing related hardware. The program can be stored in a computer-readable storage medium, such as a read-only memory, a disk, or an optical disk.

[0054] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A distillation method for improving the volatilization efficiency of magnesium chloride, characterized in that, The steps include the following: S1. After the reduction process of magnesium reducing titanium tetrachloride is completed, the distillation apparatus is assembled and then hoisted into the distillation furnace by a crane for a sealing test. S2. After the sealing test is qualified, the distillation furnace is heated. The distillation furnace is divided into zones 1, 2, 3 and 4 from top to bottom. In the first stage, the temperature of zones 1 and 4 is raised to the specified temperature and then kept at that temperature. Zone 4 is kept 300°C higher than zone 1 for a certain period of time. The heating rate in this stage is controlled at 5°C / min. S3, the second stage, heating of zones 2 and 3 is started, heating zones 2 and 3 to the specified temperature and maintaining it for a certain time, and the heating rate during this stage is controlled at 5℃ / min; S4. In the third stage, the heating in zone 1 is turned off, while zones 2, 3, and 4 continue to maintain the above temperature for a certain period of time, and the vacuum degree is controlled within the specified range. S5. In the fourth stage, zone 1 heating is activated. The temperatures of zones 1, 2, 3, and 4 are adjusted to the specified temperatures and maintained for a certain period of time before the endpoint is determined. S6. After distillation, transfer to the cooling station; In step S4, the temperature control range of zones 2, 3, and 4 is 910-920℃, the heat preservation time is controlled at 10-12h, and the vacuum degree control range is 10-15Pa. In step S5, the temperature control range of zones 1, 2, 3, and 4 is 1040-1050℃, and the heat preservation time is controlled at 50-70h.

2. The distillation method for improving the volatilization efficiency of magnesium chloride according to claim 1, characterized in that: In step S2, the temperature control range of zone 1 is 610-620℃, the temperature control range of zone 4 is 910-920℃, and the heat preservation time is controlled at 2-4 hours.

3. The distillation method for improving the volatilization efficiency of magnesium chloride according to claim 1, characterized in that: In step S3, the temperature control range of zones 2 and 3 is 910-920℃, and the heat preservation time is controlled at 5-7h.

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