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CN-121992225-A - Cold state pre-magnesium adding process method for producing titanium sponge

CN121992225ACN 121992225 ACN121992225 ACN 121992225ACN-121992225-A

Abstract

The invention discloses a cold state pre-magnesium adding process method for producing titanium sponge in the chemical field, which comprises the following steps of S1, cooling a reactor to be less than or equal to 45 ℃ after distillation, turning over and dismantling a lump-containing tank, adding a preset amount of solid magnesium ingots layer by layer through a vacuum channel of the reactor containing condensate, continuously filling argon into the reactor, S2, sealing and vacuumizing the reactor, installing a charging pipe, vacuumizing the reactor to form a negative pressure environment, S3, reducing and degassing at low temperature, maintaining a preset time after heating to a preset temperature, S4, reducing and melting condensate, maintaining a preset time after heating to the preset temperature, S5, reducing and charging, and adding The method comprises the steps of carrying out reduction reaction in a preset temperature range to generate titanium sponge, carrying out magnesium adding operation at a lower temperature of less than or equal to 45 ℃, improving safety, carrying out low-temperature degassing and reducing molten condensate subsequently to reduce production cost, and carrying out cold magnesium adding under the protection of argon to avoid oxidation of magnesium ingots and residual low-valence titanium in a reactor.

Inventors

  • CHEN CHAOGANG
  • XIANG GUILIN
  • XU HUCHENG
  • YANG XIONGGUANG
  • CHENG YONGGUO
  • LIAO YONGQIANG
  • DU JUNSHENG
  • HE YONGSHENG
  • HU GUOCHUN
  • SUN JIHUAN

Assignees

  • 攀钢集团(攀枝花)钛金属材料有限公司

Dates

Publication Date
20260508
Application Date
20260227

Claims (10)

  1. 1. The cold state pre-magnesium adding process for producing sponge titanium is characterized by comprising the following steps, S1, adding magnesium in a cold state, cooling the reactor to be less than or equal to 45 ℃ after distillation, turning over and removing a lump-containing tank, adding a preset amount of solid magnesium ingots into a vacuum channel of the reactor containing condensate layer by layer, and continuously filling argon into the reactor; s2, sealing and vacuumizing, mounting a feeding pipe, and vacuumizing the reactor to form a negative pressure environment; S3, reducing and degassing at low temperature, and maintaining the preset time after the temperature rises to the preset temperature; S4, reducing the molten condensate, and maintaining the preset time after the temperature is raised to the preset temperature; S5, reducing and feeding, adding And (3) carrying out reduction reaction in a preset temperature range to generate the titanium sponge.
  2. 2. The process for cold pre-magnesia production of titanium sponge according to claim 1, wherein the internal diameter of the vacuum channel of the reactor containing condensate in step S1 is not less than 150mm.
  3. 3. The method according to claim 1, wherein in step S1, argon is introduced into the reactor to maintain the gas pressure in the reactor at 1.5 kPa-2.0 kPa.
  4. 4. The process for cold pre-magnesia production according to claim 1, characterized in that in step S2, the vacuum in the reactor is less than or equal to-80 kPa.
  5. 5. The method according to claim 1, wherein in step S3, the temperature is raised to 300-500 ℃.
  6. 6. The method for cold pre-magnesium production according to claim 5, wherein the duration is in the range of 3h to 5h.
  7. 7. The method according to claim 1, wherein in step S4, the temperature is increased in the range of 750 ℃ to 850 ℃.
  8. 8. The method for cold pre-magnesium production according to claim 7, wherein the duration of the maintaining is in the range of 8h to 10h.
  9. 9. The method according to claim 1, wherein in step S5, the temperature is in the range of 750 ℃ to 830 ℃.
  10. 10. The cold pre-magnesium adding process for producing titanium sponge according to claim 1, wherein in step S1, the reactor is provided with a rainproof cover structure, and the rainproof cover structure is provided with a charging channel communicated with a vacuum channel of the reactor.

Description

Cold state pre-magnesium adding process method for producing titanium sponge Technical Field The invention relates to the field of chemical industry, in particular to a cold state pre-magnesium adding process method for producing titanium sponge. Background The Claoult process (combined magnesian reduction and vacuum distillation process) is a conventional method for preparing industrial mass production of titanium sponge, and is divided into full-process production and half-process production according to the production conditions of enterprises. The whole process production comprises five steps of preparing high titanium slag, preparing coarse titanium tetrachloride by chlorination, refining to obtain refined titanium tetrachloride, reducing magnesium, distilling magnesium and electrolyzing magnesium chloride, wherein the half process production only comprises the steps of reducing magnesium and distilling magnesium. In the magnesium reduction and distillation link, magnesium is used as a reducing agent and is supplemented in an online magnesium adding mode, no matter in the whole-process production (when the yield of electrolyte magnesium is insufficient) or in the semi-process production, solid magnesium ingots are manually supplemented in a high-temperature (above 500 ℃) environment, the single furnace time is 1-2 hours, the problems that operators are easy to scald in the high-temperature environment, impurities can be possibly introduced in the manual high Wen Jiamei process, the purity of the titanium sponge is not up to the standard, the magnesium adding period is long, the energy consumption is high, and the productivity is influenced easily occur. Disclosure of Invention In order to overcome the defects, the invention aims to solve the technical problems of improving quality, safety and energy consumption caused by adding magnesium in a high-temperature environment. The technical scheme adopted for solving the technical problems is as follows: The cold state pre-magnesium adding process method for producing the titanium sponge comprises the following steps: s1, adding magnesium in a cold state, cooling the reactor to be less than or equal to 45 ℃ after distillation, turning over and removing a lump-containing tank, adding a preset amount of solid magnesium ingots layer by layer through a vacuum channel of the reactor containing condensate, and continuously filling argon into the reactor; s2, sealing and vacuumizing, mounting a feeding pipe, and vacuumizing the reactor to form a negative pressure environment; S3, reducing and degassing at low temperature, and maintaining the preset time after the temperature rises to the preset temperature; S4, reducing the molten condensate, and maintaining the preset time after the temperature is raised to the preset temperature; S5, reducing and feeding, adding And (3) carrying out reduction reaction in a preset temperature range to generate the titanium sponge. Further, the inner diameter of the vacuum channel of the reactor containing condensate in the step S1 is more than or equal to 150mm. Further, in step S1, argon is filled into the reactor, so that the air pressure in the reactor is maintained at 1.5 kPa-2.0 kPa. Further, in the step S2, the vacuum degree in the reactor is less than or equal to-80 kPa. Further, in step S3, the temperature is raised in the range of 300 ℃ to 500 ℃. Further, the duration of maintenance is in the range of 3h-5h. Further, in step S4, the temperature is raised to 750 ℃ to 850 ℃. Further, the duration of maintenance is in the range of 8h-10h. Further, in step S5, the temperature ranges from 750 ℃ to 830 ℃. Further, in step S1, the reactor is provided with a rainproof cover structure, and the rainproof cover structure is provided with a charging channel communicated with the vacuum channel of the reactor. The beneficial effects of the invention are as follows: The magnesium adding operation is carried out under the condition of lower temperature less than or equal to 45 ℃, so that the scalding and fire risks caused by the traditional high-temperature operation above 500 ℃ are thoroughly avoided, the safety coefficient is obviously improved, the energy consumption for maintaining high temperature for a long time for avoiding single magnesium melting in the subsequent low-temperature degassing stage and the condensate reduction stage is reduced, the production cost is reduced, the cold magnesium adding under the protection of argon is carried out, the oxidation of residual low-valence titanium in a magnesium ingot and a reactor is effectively avoided, the impurity content of a titanium sponge product is stable, and the standard is met. Drawings FIG. 1 is a process flow diagram of the present invention; Detailed Description The invention is further described below with reference to the accompanying drawings. As shown in fig. 1, the invention provides a cold state pre-magnesium adding process method for producing titanium sponge, wh