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Method and equipment for recycling fluoride in iron-containing compound production

A technology of fluoride and compounds, which is applied in the field of fluoride recycling in the production of iron-containing compounds, can solve the problems of polluting the environment and reducing the utilization rate of fluorine-containing compounds, and achieve the effect of reducing repeated recycling

Active Publication Date: 2015-06-03
贵州万方铝化科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Now fluoride will produce a variety of wastes during the use of fluoride, such as ammonium fluoride and ammonium bifluoride as the etchant waste residue ammonium fluoroferrate and fluorine-containing carbon residue produced by the electrolytic iron production process; another example is the electrolysis process. A large amount of gas such as hydrofluoric acid and ferric trifluoride and dust such as ferric fluoride and calcium fluoride; fluorite (CaF 2 ) as a flux, so the dust contains a large amount of harmful substances such as calcium fluoride and hydrogen fluoride; magnesium and iron also produce hydrogen fluoride and iron trifluoride in the casting process; long-term storage or direct discharge of these fluorine-containing compounds will not only pollute the environment, And it reduces the utilization rate of these fluorine-containing compounds

Method used

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  • Method and equipment for recycling fluoride in iron-containing compound production
  • Method and equipment for recycling fluoride in iron-containing compound production
  • Method and equipment for recycling fluoride in iron-containing compound production

Examples

Experimental program
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Effect test

Embodiment 1

[0065] will contain Fe 2 o 3 waste with CaF 2 Mix well to get a mixture, Fe 2 o 3 with CaF 2 The particle size is below 3mm, the CaF in the resulting mixture 2 The mass percentage is 80%. Calcinate the mixture in the first reactor at 1150°C for 1 hour to generate CaO and FeF 3 , FeF 3 It is gaseous at high temperature and escapes from solid reactants. FeF that will escape 3 Introduced into the second reactor and hydrolyzed at a temperature of 1250°C to generate Fe 2 o 3 and HF gas. The HF gas produced by hydrolysis is transported to the third reactor with a polytetrafluoroethylene pipeline, and reacted with the reaction product CaO at 600°C for 2.5 hours to obtain CaF again. 2 , thus realizing CaF 2 of recycling. The reaction equation is as follows:

[0066] Fe 2 o 3 +3CaF 2 →3CaO+2FeF 3 (4)

[0067] 2FeF 3 +3H 2 O → Fe 2 o 3 +6HF (5)

[0068] CaO+2HF→CaF 2 +H 2 O (6)

Embodiment 2

[0070] Magnetite (Fe 2 o 3　 mSiO 2 ) with AlF 3 Mix well to get a mixture, magnetite and AlF 3 The particle size is below 5mm, and the AlF in the resulting mixture 3 The mass percentage is 60%. The mixture was calcined at 1300°C for 3 hours in the first reactor to generate Al 2 o 3 and gaseous FeF 3 and gaseous SiF 4 , the gaseous SiF 4 After being separated at low temperature, it is hydrolyzed to produce silicon dioxide and hydrogen fluoride. FeF 3 Escape from the solid reactant by sublimation. FeF that will escape 3 Introduced into the second reactor and hydrolyzed at 1300°C to generate Fe 2 o 3 and HF gas. The HF gas produced by hydrolysis is transported to the third reactor with polytetrafluoroethylene pipeline, and the reaction product Al 2 o 3 After reacting at 100°C for 5 hours, AlF was recovered 3 , thus achieving AlF 3 of recycling. The reaction equation is as follows:

[0071] Fe 2 o 3 +2AlF 3 →Al 2 o 3 +2FeF 3 (7)

[0072] 3SiO 2 +4A...

Embodiment 3

[0076] Will Fe 2 o 3 Coarse particles and NH 4 HF 2 Mix well, Fe 2 o 3 with NH 4 HF 2 The particle size is below 7mm, and the NH in the resulting mixture 4 HF 2 The mass percentage is 40%. The mixture was calcined at 600°C for 5 hours in the first reactor to generate NH 3 、H 2 O and FeF 3 , FeF 3 escaped from the solid. FeF that will escape 3 Introduced into the second reactor and hydrolyzed at 1100°C to generate Fe 2 o 3 and HF gas. The HF gas produced by hydrolysis is transported to the third reactor with polytetrafluoroethylene pipeline, and the reaction product NH 3 and H 2 O was reacted at 150°C for 4.5 hours to regain NH 4 HF 2 , thus achieving NH 4 HF 2 of recycling. The reaction equation is as follows:

[0077] Fe 2 o 3 +3NH 4 HF 2 →2FeF 3 +3NH 3 +3H 2 O (11)

[0078] FeF 3 +3H 2 O → Fe 2 o 3 +6HF (12)

[0079] NH 3 ·H 2 O+2HF→NH 4 HF 2 +H 2 O (13)

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Abstract

The invention relates to the field of fluoride recycling, and particularly relates to a method and equipment for recycling fluoride in iron-containing compound production. The method comprises the following steps of mixing the raw material of Fe-containing oxide with solid-state fluoride to form a mixture; calcining the mixture, wherein the Fe<3+> in the Fe-containing oxide and the F<-> in the fluoride generate a first product FeF3 gas, and the O<2-> in the Fe-containing oxide and the cation in the fluoride generate a second product; introducing water vapor into the first product and enabling reaction to form a gas-solid mixture containing solid-state Fe2O3 and gas-state HF; separating the gas-solid mixture to obtain the first gas phase containing unreacted water vapor and gas-state HF and solid-state Fe2O3; enabling the first gas phase to react with the second product to obtain solid-state fluoride again. According to the method and equipment provided by the invention, the cost is lowered through the recycling of fluoride, and the environmental pollution caused by fluoride is also avoided.

Description

technical field [0001] The invention relates to the field of fluoride recycling, in particular to a method and equipment for recycling fluoride in the production of iron-containing compounds. Background technique [0002] The fluorine in fluorine chemical products mainly comes from fluorspar, which is a non-renewable resource and a strategic resource at the same time. Efficient utilization of existing fluorine resources and conservation of existing fluorspar resources have become an important direction for the sustainable development of the fluorine chemical industry. Now fluoride will produce a variety of wastes during the use of fluoride, such as ammonium fluoride and ammonium bifluoride as the etchant waste residue ammonium fluoroferrate and fluorine-containing carbon residue produced by the electrolytic iron production process; another example is the electrolysis process. A large amount of gas such as hydrofluoric acid and ferric trifluoride and dust such as ferric fluo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/06
Inventor 章林刘瑞史春华龚龙江
Owner 贵州万方铝化科技开发有限公司
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