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Method for preparing metal titanium by taking ionic liquid as electrolyte and performing electro-deoxidization at room temperature

An ionic liquid and electrolyte technology, which is applied in the field of electro-deoxidation to prepare metal titanium, can solve the problems of uncontrolled precipitation of other impurities in the electrolyte, unclear cation diffusion, and low thermal conductivity of titanium, so as to shorten the production cycle, achieve good chemical stability, good electrical conductivity

Inactive Publication Date: 2013-03-27
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] (2) Small thermal conductivity: The thermal conductivity of titanium is small, which is one-fifth of low-carbon steel and one-twentieth of copper
[0054] At present, the deoxidation mechanism, deoxidation steps and cation diffusion of this process are still unclear, and the residue of low-valent titanium oxide in the electrolysis product cannot control the precipitation of other impurities in the electrolyte, so it has been in the laboratory research stage. If you want to ensure the quality of the product and continuous production still need to solve many problems

Method used

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  • Method for preparing metal titanium by taking ionic liquid as electrolyte and performing electro-deoxidization at room temperature
  • Method for preparing metal titanium by taking ionic liquid as electrolyte and performing electro-deoxidization at room temperature
  • Method for preparing metal titanium by taking ionic liquid as electrolyte and performing electro-deoxidization at room temperature

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Effect test

Embodiment 1

[0102] The method for preparing metal titanium by electrodeoxidation using ionic liquid as electrolyte at room temperature according to the present invention comprises the following steps:

[0103] (1) N-methylimidazole is purified by industrial grade for use. The purification process is as follows: add 200mL N-methylimidazole into a matching 500mL round bottom flask, and heat the oil bath to 140°C under the vacuum of the circulating water pump to obtain The distillate was distilled twice and sealed for use.

[0104] (2) When the power of the light wave-ultrasonic reactor is set to 160W and the temperature is 70°C, the heating time is 60s, then the heat preservation is 40s, and the ventilation is 10s as a cycle. The intermediate product, N-methylimidazole and ethyl bromide, is cycled 5 times in total. The alkane ratio is 1:1.05, and the yield reaches 96.62%.

[0105] (3) Weigh 1mol of the purified intermediate [BMIM]Br into a 250ml one-necked flask, and put 1mol of NaBF 4 Di...

Embodiment 2

[0118] (1) N-methylimidazole is industrial grade, purified for later use. The purification process is as follows: add 200mL of N-methylimidazole into a matching 500mL round bottom flask, and heat the oil bath to 140°C under the vacuum state of the circulating water pump The fractions were obtained, distilled twice, and sealed for use.

[0119] (2) When the power of the light wave-ultrasonic reactor is set to 160W and the temperature is 73°C, the heating time is 55s, then the heat preservation is 40s, and the ventilation is 10s as a cycle. The intermediate product, N-methylimidazole and ethyl bromide, is cycled 5 times in total. The ratio of alkane is 1:1.1, and the yield reaches 97%.

[0120] (3) Weigh 1mol of the purified intermediate [BMIM]Br into a 250ml one-necked flask, and put 1.2mol of NaBF 4 Dissolve in 100mL methanol, slowly add NaBF dropwise with a constant pressure dropping funnel 4 The methanol solution was magnetically stirred at room temperature for 24 hours. A...

Embodiment 3

[0126] (1) N-methylimidazole is industrial grade, purified for later use. The purification process is as follows: add 200mL of N-methylimidazole into a matching 500mL round bottom flask, and heat the oil bath to 140°C under the vacuum state of the circulating water pump The fractions were obtained, distilled twice, and sealed for use.

[0127] (2) When the power of the light wave-ultrasonic reactor is set to 160W and the temperature is 75°C, the heating time is 66s, then the heat preservation is 35s, and the ventilation is 10s as a cycle, and a total of 5 cycles are obtained to obtain the intermediate product, N-methylimidazole and ethyl bromide The ratio of alkane is 1:1.08, and the yield reaches 95%.

[0128] (3) Weigh 1mol of the purified intermediate [BMIM]Br into a 250ml one-necked flask, and put 1.03mol of NaBF 4 Dissolve in 100mL methanol, slowly add NaBF dropwise with a constant pressure dropping funnel 4 The methanol solution was magnetically stirred at room tempera...

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Abstract

The invention relates to a method for preparing metal titanium by electro-deoxidization and specifically relates to the method for preparing the metal titanium by taking ionic liquid as an electrolyte and performing the electro-deoxidization at room temperature. The method comprises the following steps: performing electrolysis at the room temperature by taking the ionic liquid as the electrolyte, taking graphite as an anode and taking a prepared cathode as a cathode, wherein the ionic liquid is prepared by firstly preparing an intermediate of the ionic liquid from N-methylimidazole and halogenated alkane by adopting a light wave-ultrasonic wave synthesis method and further reacting the intermediate of the ionic liquid with sodium tetrafluoroborate for preparation. The method disclosed by the invention has the advantages of convenience in operation, high reaction speed, high efficiency and high yield, as well as high product purity and capability of reducing production period, so that the method is an environment-friendly, green and low-energy-consumption new method for preparing metal titanium by electro-deoxidization.

Description

technical field [0001] The invention relates to a method for preparing metallic titanium by electrodeoxidation, in particular to a method for preparing metallic titanium by electrodeoxidation at room temperature using ionic liquid as an electrolyte. Background technique [0002] Ionic liquids (Room Temperature Ionic Liquids) are ionic compounds composed of organic cations and inorganic or organic anions, most of which are liquid at room temperature. Compared with traditional high-temperature molten salts, they are also called "room temperature molten salts", abbreviated as RTILs. Within a certain temperature range, only anions and cations exist in ionic liquids. Ordinary ionic compounds are generally solid at room temperature, and the ionic bonds are relatively strong, so that anions and cations can only vibrate on the crystal lattice, and cannot rotate or translate. Therefore, Generally, ionic compounds have relatively high melting points. Compared with traditional organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C3/28
Inventor 张丽鹏于先进穆洁尘王捷梁寒冰张德超陈恩泽
Owner SHANDONG UNIV OF TECH
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