阅读说明：本技术 海绵钛生产中用底排式还原罐制取高纯镁的方法 (Method for preparing high-purity magnesium by using bottom discharge type reduction tank in titanium sponge production ) 是由 黄子良 姜宝伟 于 2020-05-14 设计创作，主要内容包括：本发明公开的是海绵钛生产技术领域的一种海绵钛生产中用底排式还原罐制取高纯镁的方法,包括以下步骤：先将生产单炉海绵钛用的全部镁原料加入底排式还原罐内,然后将镁原料全部熔化成液态并升温至700～800℃；然后向液镁中缓慢加入四氯化钛,四氯化钛加入量为生产单炉海绵钛所需四氯化钛总量的0.3～1.5％；最后将液镁保温静置一段时间后,打开底排式还原罐底部阀门,排出还原反应所生成的氯化镁总量的50～80％,液镁中的杂质随氯化镁熔体从还原罐底部排出,镁净化完成。整个处理方法简单,处理过程安全可靠,且不需另外增加处理设施,成本较低。(The invention discloses a method for preparing high-purity magnesium by using a bottom discharge type reduction tank in titanium sponge production, which belongs to the technical field of titanium sponge production and comprises the following steps: firstly, adding all magnesium raw materials for producing single-furnace titanium sponge into a bottom discharge type reduction tank, then completely melting the magnesium raw materials into a liquid state, and heating to 700-800 ℃; slowly adding titanium tetrachloride into the liquid magnesium, wherein the adding amount of the titanium tetrachloride is 0.3-1.5% of the total amount of the titanium tetrachloride required for producing the single-furnace titanium sponge; and finally, after the liquid magnesium is kept warm and stands for a period of time, opening a valve at the bottom of the bottom discharge type reduction tank, discharging 50-80% of the total amount of magnesium chloride generated by the reduction reaction, discharging impurities in the liquid magnesium from the bottom of the reduction tank along with magnesium chloride melt, and finishing magnesium purification. The whole treatment method is simple, the treatment process is safe and reliable, no additional treatment facilities are needed, and the cost is low.)

1. The method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge is characterized by comprising the following steps of:

a. firstly, adding all magnesium raw materials for producing single-furnace titanium sponge into a bottom discharge type reduction tank, then completely melting the magnesium raw materials into a liquid state, and heating to 700-800 ℃;

b. slowly adding titanium tetrachloride into the liquid magnesium, wherein the adding amount of the titanium tetrachloride is 0.3-1.5% of the total amount of the titanium tetrachloride required for producing the single-furnace titanium sponge;

c. and (3) after the liquid magnesium is kept at the temperature and is kept stand for a period of time, opening a valve at the bottom of the bottom discharge type reduction tank, discharging 50-80% of the total amount of magnesium chloride generated by the reduction reaction, discharging impurities in the liquid magnesium from the bottom of the reduction tank along with magnesium chloride melt, and finishing magnesium purification.

2. The method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge as claimed in claim 1, which is characterized in that: the method for adding titanium tetrachloride into the bottom discharge type reduction tank is the same as the conventional adding method in the production of sponge titanium, and the reduction tank is sealed and protected by argon.

3. The method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge as claimed in claim 1, which is characterized in that: and adding titanium tetrachloride into the bottom discharge type reduction tank for 60-120 minutes, and uniformly feeding according to the adding amount and time.

4. The method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge as claimed in claim 1, which is characterized in that: and standing the liquid magnesium for 30-180 minutes.

Technical Field

The invention relates to the technical field of sponge titanium production, in particular to a method for preparing high-purity magnesium by using a bottom discharge type reduction tank in sponge titanium production.

Background

The magnesium raw material often contains harmful impurities such as iron, aluminum, silicon, manganese and the like, and when the magnesium thermal method is used for producing the titanium sponge, the impurities can reduce the quality of the titanium sponge product, and magnesium needs to be refined for producing high-quality titanium sponge. In a general magnesium refining method, a refining flux is added into liquid magnesium for refining in a special magnesium refining furnace (or a crucible furnace), but the refining method cannot effectively remove impurities such as iron, aluminum, silicon, manganese and the like in metal magnesium. At present, there is a method for refining magnesium by removing impurities such as iron, aluminum, silicon, manganese and the like in magnesium by adopting a metallothermic reduction method, for example, liquid magnesium is refined by directly adding titanium sponge particles, the refining effect of the method is related to the size of the adopted titanium sponge particles, the refining temperature, whether the titanium sponge particles are uniformly stirred or not, the quality of the titanium sponge, and the like, and the process operation is complex. On the other hand, the production of the titanium sponge is divided into a type I semi-combination method (combination method) and an inverted U-shaped combination method flow, and the reduction tank adopted by the furnace I method is divided into two modes of discharging magnesium chloride and discharging magnesium chloride from the bottom.

Disclosure of Invention

In order to overcome the defects of complex process operation, high cost and the like of the existing method for purifying magnesium, the invention aims to solve the technical problems that: provides a simple, convenient and low-cost method for preparing high-purity magnesium in the production of titanium sponge.

The technical scheme adopted by the invention for solving the technical problems is as follows:

the method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge comprises the following steps:

a. firstly, adding all magnesium raw materials for producing single-furnace titanium sponge into a bottom discharge type reduction tank, then completely melting the magnesium raw materials into a liquid state, and heating to 700-800 ℃;

b. slowly adding titanium tetrachloride into the liquid magnesium, wherein the adding amount of the titanium tetrachloride is 0.3-1.5% of the total amount of the titanium tetrachloride required for producing the single-furnace titanium sponge;

c. and (3) after the liquid magnesium is kept at the temperature and is kept stand for a period of time, opening a valve at the bottom of the bottom discharge type reduction tank, discharging 50-80% of the total amount of magnesium chloride generated by the reduction reaction, discharging impurities in the liquid magnesium from the bottom of the reduction tank along with magnesium chloride melt, and finishing magnesium purification.

Furthermore, the method for adding titanium tetrachloride into the bottom discharge type reduction tank is the same as the conventional adding method in the production of sponge titanium, and the reduction tank is sealed and protected by argon.

Further, the time for adding titanium tetrachloride into the bottom discharge type reduction tank is 60-120 minutes, and uniform feeding is carried out according to the adding amount and time.

Further, the standing and heat preservation time of the liquid magnesium is 30-180 minutes.

The invention has the beneficial effects that: titanium tetrachloride added into liquid magnesium reacts with magnesium to generate fine sponge titanium particles and magnesium chloride melt, the fine sponge titanium particles and the magnesium chloride melt gradually settle to the bottom of a tank from the surface of the liquid magnesium, the surface of the sponge titanium particles continuously adsorbs metal impurities or further generates insoluble intermetallic compounds in the settling process, and when the magnesium chloride melt is discharged from the bottom of a reduction tank, the sponge titanium particles adsorbing the metal impurities and the insoluble intermetallic compounds are discharged along with the magnesium chloride, so that the aim of purifying the magnesium is fulfilled.

Detailed Description

The present invention is further described below.

The method for preparing high-purity magnesium by using the bottom discharge type reduction tank in the production of the titanium sponge comprises the following steps:

a. firstly, adding all magnesium raw materials for producing single-furnace titanium sponge into a bottom discharge type reduction tank, then completely melting the magnesium raw materials into a liquid state, and heating to 700-800 ℃;

b. slowly adding titanium tetrachloride into the liquid magnesium, wherein the adding amount of the titanium tetrachloride is 0.3-1.5% of the total amount of the titanium tetrachloride required for producing the single-furnace titanium sponge;

c. and (3) after the liquid magnesium is kept at the temperature and is kept stand for a period of time, opening a valve at the bottom of the bottom discharge type reduction tank, discharging 50-80% of the total amount of magnesium chloride generated by the reduction reaction, discharging impurities in the liquid magnesium from the bottom of the reduction tank along with magnesium chloride melt, and finishing magnesium purification.

The principle of the method is as follows: firstly, melting a magnesium raw material into a liquid state, heating to 700-800 ℃, and enabling magnesium to react with titanium tetrachloride added subsequently; then, when titanium tetrachloride is slowly added, the titanium tetrachloride reacts with magnesium to generate fine titanium sponge particles and magnesium chloride melt, the titanium sponge particles and the magnesium chloride melt are gradually settled from the surface of liquid magnesium to the bottom of a tank because the density of the titanium sponge particles is larger than that of the magnesium, and the surfaces of the titanium sponge particles continuously adsorb metal impurities or further generate insoluble intermetallic compounds in the settling process; after the charging is finished, the mixture is kept warm and kept stand for a period of time, so that the titanium sponge particles adsorbing the metal impurities and the magnesium chloride melt are completely settled at the bottom of the furnace, finally the magnesium chloride melt is discharged from the bottom of the reduction tank, and the titanium sponge particles adsorbing the metal impurities and the indissolvable intermetallic compounds are discharged along with the magnesium chloride, thereby achieving the purpose of purifying the magnesium. The whole treatment method is simple, the treatment process is safe and reliable, no additional treatment facilities are needed, and the cost is low.

According to the purity of the commonly used magnesium raw material at present, the adding amount of titanium tetrachloride is more appropriate to be 0.3-1.5% of the total amount of titanium tetrachloride required for producing the titanium sponge of a single furnace, metal impurities cannot be sufficiently adsorbed if the adding amount of titanium tetrachloride is too small, and the purification time is prolonged if the adding amount of titanium tetrachloride is too much. The method for adding titanium tetrachloride is the same as the conventional method for adding titanium sponge, the reduction tank is sealed and protected by argon, and the contact reaction of liquid magnesium and air is avoided. The feeding speed is determined according to the feeding amount and the feeding time, and is preferably controlled to be 60-120 minutes, so that the metal adsorption effect can be improved. When the discharge amount of the magnesium chloride melt is determined, according to test summary, 50-80% of the total amount of magnesium chloride generated by the reduction reaction is properly discharged, and most of metal impurities can be discharged along with the magnesium chloride. In order to ensure that the metal impurities can be fully settled, the standing and heat preservation time of the liquid magnesium is preferably 30-180 minutes.

The following examples are further illustrated