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Recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as intermediate raw material

A technology of potassium fluorotitanate and potassium cryolite, which is applied in the direction of aluminum fluoride, alkali metal fluoride, and improvement of process efficiency, can solve the problems of unfavorable environmental protection, harsh reaction conditions, and high production cost of chlorine gas, and achieve full realization Recycling, short production cycle, and the effect of reducing the overall cost of production

Active Publication Date: 2012-07-18
SONGYAN METALLURGICAL MATERIALS (QUANNAN) CO LTD
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Therefore, the existing technology uses titanium tetrachloride as an intermediate raw material to prepare sponge titanium and has disadvantages such as complex process, harsh reaction conditions, high equipment investment requirements, long production cycle, high production cost, and the use of chlorine is not conducive to environmental protection.

Method used

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  • Recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as intermediate raw material
  • Recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as intermediate raw material
  • Recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as intermediate raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Put 1 ton of ilmenite concentrate powder in a reaction kettle, add 1.5 tons of hydrofluoric acid with a volume fraction of 30%, and fully react at 120°C to generate fluorotitanic acid. After the fluorotitanic acid is cooled, add the mass fraction 4 tons of 10% potassium sulfate solution, react fully to form potassium fluotitanate precipitate, centrifuge, rinse, dry to obtain potassium fluotitanate, weigh; put potassium fluotitanate in another reactor, vacuumize Introduce argon protection, heat up to 800°C, slowly drop aluminum liquid into the reactor according to the reaction ratio, stir rapidly, react for 5 hours, and generate sponge titanium and potassium cryolite, open the reactor cover, and use a siphon pump to pump out the potassium in the upper layer Cryolite, the titanium sponge in the lower layer is purified by vacuum distillation at 1000°C to obtain purified titanium sponge; after cooling, the potassium cryolite is crushed, weighed, and concentrated sulfuric aci...

Embodiment 2

[0027] Put 1 ton of ilmenite concentrate powder in a reaction kettle, add 1.5 tons of hydrofluoric acid with a volume fraction of 30%, and fully react at 120°C to generate fluorotitanic acid. After the fluorotitanic acid is cooled, add the mass fraction 4 tons of 10% potassium sulfate solution, fully reacted to form potassium fluotitanate precipitate, centrifuged, rinsed, dried to obtain potassium fluotitanate, weighed; weighed aluminum according to the reaction ratio and put it in another reactor, vacuumized Afterwards, the argon gas protection was introduced, and the temperature was raised to 800°C. Add dried potassium fluorotitanate into the reactor, stir rapidly, and react for 5 hours to generate sponge titanium and potassium cryolite. Open the reactor cover, and use a siphon pump to draw out the upper layer Potassium cryolite, the sponge titanium in the lower layer is purified by vacuum distillation at 1000°C to obtain purified sponge titanium; the potassium cryolite is br...

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Abstract

The invention discloses a recycling preparation method for producing titanium sponge and co-producing potassium cryolite with potassium fluotitanate as an intermediate raw material. The method comprises the following steps of: A) adding hydrofluoric acid to titaniferous iron concentrates to react to generate fluotitanic acid; B) adding potassium sulfate to fluotitanic acid to react to generate potassium fluotitanate; C) putting potassium fluotitanate into a reactor and adding aluminium to react to generate titanium sponge potassium cryolite; or putting aluminium into the reactor and adding potassium fluotitanate to react to generate titanium sponge potassium cryolite; D) extracting potassium cryolite, feeding the extracted potassium cryolite and concentrated sulfuric acid into a rotary reaction kettle to react to generate hydrogen fluoride, potassium sulfate and aluminium potassium sulfate and collecting hydrogen fluoride and dissolving hydrogen fluoride in water to obtain hydrofluoric acid water solution; and E) recycling the obtained hydrofluoric acid water solution to the step A to be used for extracting the titaniferous iron concentrates. The method has the beneficial effects of recycling the byproduct potassium cryolite, shortening the preparation process flows of titanium sponge, lowering the comprehensive production cost, improving the production efficiency and reducingthe environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of titanium sponge, in particular to a cyclic preparation method for producing titanium sponge by using potassium fluotitanate as an intermediate raw material and synchronously producing potassium cryolite. Background technique [0002] Ilmenite concentrate is the most important mineral raw material for extracting titanium. The existing preparation method of sponge titanium uses ilmenite concentrate as the starting material, and obtains titanium-rich material through reduction smelting method, chlorination smelting method, pre-reduction hydrochloric acid leaching method or pre-reduction sulfuric acid leaching method, and then uses titanium-rich material and coke Titanium tetrachloride produced by the reaction of chlorine gas at a high temperature of about 1000°C is used as an intermediate raw material, and titanium sponge is prepared by magnesia thermal reduction method (Kroll method) or sodium thermal redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/12C01F7/54
CPCC01D3/02C22B34/12C22B34/1277C01F7/54Y02P10/20
Inventor 陈学敏余跃明叶清东杨军周志陈昕旖
Owner SONGYAN METALLURGICAL MATERIALS (QUANNAN) CO LTD
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