Titanizing method for titanium sponge production reactor

Abstract

The invention relates to the technical field of titanium sponge production, in particular to a titanium sponge production reactor titanizing method. A titanium powder titanizing stage: uniformly laying titanium powder on the inner wall of the reactor, and carrying out preliminary diffusion coating in an inert atmosphere; and a distillation titanizing stage: placing sponge titanium on a prefabricated titanizing frame, and carrying out a distillation process with a period of 50 hours at 900-1000 DEG C to promote the titanium element to deeply permeate and form a stable titanium-iron alloy layer with the matrix iron. By strengthening the compactness and stability of the titanium alloy layer on the inner surface of the reactor, the iron dissolution amount is reduced by 30-50% from the source, it is ensured that the Fe content of a sponge titanium product stably reaches the standard (smaller than or equal to 0.03%), meanwhile, the process cost is controllable, complex equipment transformation is not needed, operation is easy, and the temperature control stages are few.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of titanium sponge production, and particularly relates to a method for titanium infiltration of a titanium sponge production reactor. BACKGROUND

[0002] When a newly commissioned reactor is directly used for titanium sponge production, since its material is mainly steel, under a high-temperature magnesium reduction atmosphere (usually maintained at 800-1000°C), the iron element on the internal surface will accelerate precipitation due to thermodynamic instability. Uncontrolled iron ions (Fe) diffuse and migrate to the surface area of the titanium lump and react with the titanium generated by reduction to form a dense and hard titanium-iron alloy (Ti-Fe) shell layer. This hard shell seriously wraps the main structure of the titanium lump, hindering the uniform growth and purification process of the titanium sponge. This phenomenon leads to a significant excess of iron content in the final product (usually exceeding 0.05% of the industry standard), not only reducing the grade of titanium sponge, but also possibly causing product unqualified problems, significantly weakening its market value and subsequent application performance.

[0003] The traditional single titanium powder infiltration method has limited effect on new reactors, as this method can only form a thin layer of protection and cannot effectively inhibit the precipitation of iron in the high-activity surface area, so process technology breakthroughs are urgently needed.

[0004] In particular, a surface treatment process specifically for newly commissioned reactors, particularly a combined titanium infiltration process for titanium sponge production reactors, needs to be developed.

[0005] This process aims to control the dissolution rate and migration path of iron (Fe) impurities in new reactors through multi-material synergistic surface modification, such as combining titanium powder with rare earth element coatings, forming a dense passivation layer, which will significantly reduce the formation of titanium-iron alloy hard shell, improve the purity of titanium sponge products to below 0.03%, and ensure the stable output of high-grade titanium sponge.

[0006] On August 3, 2025, a search was conducted in the China Patent Publication Database with "titanium and low temperature and high temperature and infiltration and inner wall and inert gas and distillation" as the abstract keywords, with the synonym expansion option selected, and no relevant literature was found.

[0007] 2025-08-03, with "titanium and low temperature and high temperature and infiltration and inner wall and inert gas and distillation" in China CNKI abstract retrieval, single sword; shen junyu; huang chunming; Luo Lin; Zhao Mingquan; Zhao Yirong; Xie Yuanfang et al published "a method for infiltrating titanium powder into titanium sponge production reactor and its application", the conventional titanium powder infiltration method is to brush a certain particle size titanium powder on the inner wall surface of the new reactor after acid dipping, water washing and drying, and then put it into the heating equipment, and go through the low temperature degassing and high temperature sintering process, so that the titanium powder adheres to the inner wall surface of the new reactor. Because the titanium powder required for titanium infiltration is not easy to obtain, especially when the titanium powder is sieved, the labor intensity and material loss are large, the cost is high, and the titanium powder is easy to be polluted by oxygen and chlorine during sieving, the titanium powder particles are not uniform, and the flowability and adhesion are poor. The present application provides a method for infiltrating titanium powder into a new reactor for producing titanium sponge. After leak detection, acid dipping, water washing and drying, the inner wall surface layer of the new reactor for producing titanium sponge is uniformly brushed with titanium hydride powder with a thickness of 0.08-0.5mm and a particle size diameter of not more than 0.043mm. Put the brushed new reactor into the heating equipment, and go through 2-5 hours of 150-250℃ low temperature degassing under vacuum, then go through medium temperature degassing, the temperature is controlled as 250-350℃, 350-550℃ and 550-700℃ in three temperature sections in turn, and each temperature is kept for 1-2 hours. After dehydrogenation, inert gas is input, and then go through 8-15 hours of 960-980℃ high temperature sintering.

[0008] The problem of the above technology is that temperature control is difficult, there are too many temperature stages, and complex operation is required. SUMMARY

[0009] The purpose of the application is to provide a titanium sponge production reactor infiltration method with better effect, and the specific purposes are shown in the multiple substantial technical effects of the specific implementation part.

[0010] In order to achieve the above purpose, the present application adopts the following technical scheme:

[0011] A titanium sponge production reactor infiltration method, characterized in that a "titanium powder infiltration + distillation titanium infiltration double combination process" is adopted, which specifically includes:

[0012] Titanium powder infiltration stage: uniformly lay titanium powder on the inner wall of the reactor, and carry out preliminary infiltration in inert atmosphere;

[0013] Distillation titanium infiltration stage: place the titanium sponge on the pre-prepared titanium infiltration frame, and go through a 50h distillation process at 900-1000℃ to promote the deep penetration of titanium element and the formation of stable titanium-iron alloy layer with the matrix iron.

[0014] The further technical scheme of the present application is that, through the synergistic effect of low-temperature titanium powder pre-plating and high-temperature vapor alloying, a uniform-thickness and metallurgical-bonded Fe-Ti alloy barrier layer is generated on the inner surface of the reactor.

[0015] The further technical scheme of the present application is that, the titanium infiltration frame is placed in the sponge titanium production reactor.

[0016] The further technical scheme of the present application is that, the titanium infiltration frame is made of high-temperature-resistant material.

[0017] The further technical scheme of the present application is that, the method for uniformly laying the titanium powder is to add the titanium powder into water and polyvinyl alcohol, and then brush the whole liquid form.

[0018] The present application with the above technical scheme has the following beneficial effects compared with the prior art: by strengthening the density and stability of the titanium alloy layer on the inner surface of the reactor, the iron dissolution amount is reduced by 30-50% from the source, the Fe content of the sponge titanium product is ensured to be stable and up to standard (≤0.03%), the process cost is controllable, complex equipment modification is not needed, the operation is simple, and the temperature control stage is less. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to further illustrate the present application, the following further illustrates the present application in combination with the drawings:

[0020] Figure 1 The present application is a process flowchart. DETAILED DESCRIPTION

[0021] The present application is further illustrated below in combination with the drawings and specific embodiments, and it should be understood that the following specific embodiments are only used to illustrate the present application and are not used to limit the scope of the present application.

[0022] In view of the initial Fe pollution problem of the new reactor, the present application provides an optimized combined titanium infiltration process,

[0023] Technical scheme:

[0024] The core is to adopt the dual combined process of titanium powder infiltration + distillation titanium infiltration, which specifically includes:

[0025] Titanium powder infiltration stage: uniformly lay titanium powder on the inner wall of the reactor, and carry out preliminary infiltration under inert atmosphere;

[0026] Distillation titanium infiltration stage, place the sponge titanium on the prefabricated titanium infiltration frame, and carry out a distillation process of about 50h at 900-1000℃, so as to promote the deep penetration of titanium element and form a stable titanium-iron alloy layer with the base iron.

[0027] The combined process generates a uniform and metallurgical bonded Fe-Ti alloy barrier layer on the inner surface of the reactor by the synergistic effect of low-temperature titanium powder pre-plating and high-temperature vapor alloying, significantly improving the anti-iron dissolution capacity.

[0028] Sharp reduction in iron dissolution: The new reactor treated by the combined process has a 30-50% reduction in the first production of the inner wall Fe dissolution compared with the traditional single titanium powder infiltration method.

[0029] Product purity guarantee: Source control makes the Fe content of sponge titanium products stable at ≤0.03%;

[0030] Alloy coating inhibition: The Ti-Fe alloy hard shell formation area on the titanium slug surface is reduced by more than 70%, ensuring the uniformity of the titanium slug structure.

[0031] The inert gas is preferably argon.

[0032] The above shows and describes the basic principles, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited by the above examples, and the above examples and descriptions in the specification are only to illustrate the principles of the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the present application.

Claims

1. A method for titanium diffusion into a reactor for producing sponge titanium, characterized in that, The process employs a "dual combination of titanium powder titanium diffusion and distillation titanium diffusion," specifically including: Titanium powder infiltration stage: Titanium powder is evenly spread on the inner wall of the reactor and preliminary infiltration is carried out under an inert atmosphere; Distillation titanium diffusion stage: Sponge titanium is placed on a prefabricated titanium diffusion rack and distilled at 900-1000℃ for a cycle of 50 hours to promote deep penetration of titanium elements and form a stable titanium-iron alloy layer with the base iron.

2. The method for titanium diffusion into a sponge titanium production reactor as described in claim 1, characterized in that, Through the synergistic effect of low-temperature titanium powder pre-plating and high-temperature steam alloying, a uniform and metallurgically bonded Fe-Ti alloy barrier layer is generated on the inner surface of the reactor.

3. The method for titanium diffusion into a sponge titanium production reactor as described in claim 1, characterized in that, The titanium infiltration frame is placed in the titanium sponge production reactor.

4. The method for titanium diffusion into a sponge titanium production reactor as described in claim 1, characterized in that, The titanium-doped frame is made of high-temperature resistant material.

5. The method for titanium diffusion into a sponge titanium production reactor as described in claim 1, characterized in that, The method for evenly spreading titanium powder involves adding titanium powder to water and polyvinyl alcohol, creating a liquid state, and then brushing it on.

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