CN112126800A

CN112126800A - Pre-pumping method for assembling reactor and large cover in titanium sponge production

Info

Publication number: CN112126800A
Application number: CN202011082338.8A
Authority: CN
Inventors: 舒煜; 龚小玲; 李金泽
Original assignee: Zunyi Titanium Industry Co Ltd
Current assignee: Zunyi Titanium Industry Co Ltd
Priority date: 2020-10-12
Filing date: 2020-10-12
Publication date: 2020-12-25

Abstract

The pre-pumping method for assembling the reactor and the large cover in the production of the titanium sponge comprises the following steps: after the reactor and the large cover are assembled, connecting pipelines, closing a valve, opening a clamp, starting a mechanical pump, evacuating a cold end system formed by the reactor and the large cover, keeping the reading of a vacuum meter of the cold end system at-75 to-90 kilopascals, evacuating for 24 hours, then stopping the mechanical pump, detecting the leakage by using a Mach vacuum gauge, and detecting the leakage in the vacuum degree range of 0 to 3 pascals, wherein the leakage is qualified; and after the leakage detection is qualified, opening a valve, starting a mechanical pump, enabling hot air of the heat supply device to enter a cold end system assembled by the reactor and the large cover through a conveying pipe, keeping the reading of a vacuum meter of the cold end system at-75 to-90 kPa, heating for 6 hours to remove moisture, then closing the valve, simultaneously cutting off a vacuum hose pipeline through a clamp, and stopping the mechanical pump to finish the pre-pumping work. The invention can completely remove the water of chloride and low-price substances, the early stage vacuum degree of the distillation stage is not influenced, and the vacuum system is not polluted, so that the product quality is ensured.

Description

Pre-pumping method for assembling reactor and large cover in titanium sponge production

Technical Field

The invention relates to a pre-pumping method for assembling a reactor and a large cover in the production of titanium sponge.

Background

At present, large-scale titanium sponge production at home and abroad adopts a magnesium method to produce titanium sponge, a furnace type adopts a combination method, namely a hot end system and a cold end system, wherein the hot end system and the cold end system are formed by assembling a reactor and a large cover, when in reduction, fine titanium tetrachloride is added into the hot end system at a high temperature state to react with liquid fine magnesium contained in the reactor to prepare metal titanium and magnesium chloride, then the cold end system is connected beside the hot end system through a passage according to the physical characteristics of various components of distillate, low-price titanium, magnesium chloride and magnesium in the reactor of the hot end system are distilled into the reactor of the cold end system at a high temperature and a high vacuum state, the pure titanium sponge is obtained by the hot end system, and the low-price titanium, magnesium chloride and magnesium are collected in the reactor of the cold end system. After distillation is finished, the cold end system is hung into the heating furnace to become a new hot end system. In the titanium sponge production, reactor and big lid belong to important equipment, after the titanium sponge reduction, before carrying out the distillation, preparation process must clear up, assemble into cold junction system, work such as sampling leak in advance to the attachment on reactor and big lid surface, just gets into distillation system's cold junction. The method is recycled until the reactor or the large cover is scrapped, but the reactor and the large cover are used repeatedly, a large amount of low-valent substances and chlorides remained in production are adsorbed frequently, the chlorides and the low-valent substances have strong water absorption and are easy to hydrolyze, and a large amount of chlorides and low-valent substances cannot be removed thoroughly in the cleaning process of the preparation process, so that the vacuum degree at the early stage of the distillation stage is influenced and a vacuum system is polluted along with the investment of the reactor and the large cover in production after the chlorides and the low-valent substances are hydrolyzed; residual low-valent substances and chlorides affect the quality of products after absorbing water.

Disclosure of Invention

The invention aims to solve the problems that in the prior art, a great amount of chlorides and low-price substances cannot be thoroughly removed during cleaning in a preparation process, so that the early vacuum degree of a distillation stage is influenced and a vacuum system is polluted along with the investment of a reactor and a large cover in production after the chlorides and the low-price substances are hydrolyzed; but also the residual low-price substances and chlorides affect the quality of the product after absorbing water.

The technical scheme of the invention is as follows:

the pre-pumping method for assembling the reactor and the large cover in the production of the titanium sponge comprises a pre-pumping device, wherein the pre-pumping device consists of a conveying pipe 1, a valve 2, a magnesium chloride pipe 3, a reactor 4, a large cover 5, a clamp 6, a vacuum hose 7, a pumping pipe 8, a mechanical pump 9 and a heat supply device 10;

the method comprises the following steps: after the reactor 4 and the large cover 5 are assembled, connecting pipelines, closing the valve 2, opening the clamp 6, starting the mechanical pump 9, evacuating a cold end system formed by the reactor 4 and the large cover 5 to ensure that the reading of a vacuum meter of the cold end system is kept at minus 75 to minus 90 kilopascals for 24 hours, then stopping the mechanical pump 9, detecting the leakage by using a Mach vacuum gauge, and ensuring that the vacuum degree of the Mach vacuum gauge is reduced within the range of 0 to 3 pascals to be qualified; and after the leakage detection is qualified, opening the valve 2, starting the mechanical pump 9, enabling hot air of the heat supply device 10 to enter a cold end system assembled by the reactor 4 and the large cover 5 through the conveying pipe 1, keeping the reading of a vacuum meter of the cold end system at-75 to-90 kPa, heating for 6 hours to remove moisture, then closing the valve 2, simultaneously cutting off a vacuum hose 7 pipeline through the clamp 6, and stopping the mechanical pump 9, thus finishing the pre-pumping work.

The invention has the following specific advantages and positive effects:

the invention can completely remove the water of chloride and low-price substances, the early stage vacuum degree of the distillation stage is not influenced, and the vacuum system is not polluted, so that the product quality is ensured.

Drawings

FIG. 1 is a schematic view of an apparatus used in the present invention.

In the figure: 1-conveying pipe, 2-valve, 3-magnesium chloride pipe, 4-reactor, 5-large cover, 6-clamp, 7-vacuum hose, 8-evacuation pipe, 9-mechanical pump and 10-heat supply device.

Detailed Description

The present invention will be described in further detail with reference to the drawings, but it should not be construed that the scope of the subject matter of the present invention is limited to the following embodiments, and various modifications, substitutions and alterations made based on the knowledge and conventional practices of the ordinary skill in the art are included in the scope of the present invention without departing from the technical spirit of the present invention.

As shown in figure 1, the pre-pumping method for assembling the reactor and the large cover in the production of the titanium sponge comprises a pre-pumping device, wherein the pre-pumping device consists of a conveying pipe 1, a valve 2, a magnesium chloride pipe 3, a reactor 4, a large cover 5, a clamp 6, a vacuum hose 7, an evacuation pipe 8, a mechanical pump 9 and a heat supply device 10;

Claims

1. The pre-pumping method for assembling the reactor and the large cover in the production of the titanium sponge comprises a pre-pumping device, wherein the pre-pumping device consists of a conveying pipe (1), a valve (2), a magnesium chloride pipe (3), a reactor (4), the large cover (5), a clamp (6), a vacuum hose (7), an evacuation pipe (8), a mechanical pump (9) and a heat supply device (10);

the method is characterized in that: the method comprises the following steps: after the reactor (4) and the large cover (5) are assembled, connecting pipelines, closing a valve (2), opening a clamp (6), starting a mechanical pump (9), evacuating a cold end system formed by the reactor (4) and the large cover (5), keeping the reading of a vacuum meter of the cold end system at-75 to-90 kilopascals, evacuating for 24 hours, then stopping the mechanical pump (9), detecting leakage by using a Mach vacuum gauge, and detecting the qualified leakage when the vacuum degree of the Mach vacuum gauge is reduced within the range of 0 to 3 pascals; and after the leakage detection is qualified, opening the valve (2), starting the mechanical pump (9), allowing hot air of the heat supply device (10) to enter a cold end system assembled by the reactor (4) and the large cover (5) through the conveying pipe (1), keeping the reading of a vacuum meter of the cold end system at-75 to-90 kPa, heating for 6 hours to remove moisture, then closing the valve (2), simultaneously cutting off a vacuum hose (7) pipeline through the clamp (6), and stopping the mechanical pump (9), thus completing the pre-pumping work.