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Method for preparing hydrogen fluoride (HF) and white carbon black by treating fluosilicic acid (H2SiF6) via organic alkali

A technology of fluosilicic acid and organic base, applied in the field of efficient utilization of by-product dilute fluosilicic acid resources, can solve problems such as unreasonable utilization of phosphoric acid by-product fluosilicic acid, and achieve the effect of novel process routes

Active Publication Date: 2013-12-25
云天化集团有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the existing unreasonable technical defects in the use of fluorosilicic acid, a by-product of phosphate fertilizer and wet-process phosphoric acid, and provide a method for producing hydrogen fluoride and white carbon black by utilizing fluorosilicic acid, a by-product of phosphate fertilizer enterprises, which can efficiently A Method of Using Phosphate Fertilizer to Produce By-Product Fluorosilicic Acid

Method used

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  • Method for preparing hydrogen fluoride (HF) and white carbon black by treating fluosilicic acid (H2SiF6) via organic alkali
  • Method for preparing hydrogen fluoride (HF) and white carbon black by treating fluosilicic acid (H2SiF6) via organic alkali

Examples

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Effect test

Embodiment 1

[0031] Mix 100 g of fluorosilicic acid solution with 10% mass fraction and 80 g of tri-n-heptylamine, gradually increase the temperature to 60 ℃, and mix and stir for 2 h. Then, the aqueous phase was removed by liquid separation, 71 g of tripropylamine was added to the organic phase, reacted for 3 h, and the solid and the filtrate were obtained by suction filtration. The solid is washed with water and dried to obtain white carbon black. The filtrate was distilled out of all the tripropylamine in the system at a temperature of 90°C under a pressure of 200 mabr in the system, and then the temperature of the system was maintained at the same pressure, and the temperature was increased to 150°C to obtain HF.

Embodiment 2

[0033] Mix 100 g of fluorosilicic acid solution with 10% mass fraction and 80 g of tri-n-heptylamine, gradually increase the temperature to 60 ℃, and mix and stir for 2 h. Then, the water phase was removed by liquid separation, 30 g of trimethylamine was added to the organic phase, and the reaction was carried out for 1.5 h, and the solid and the filtrate were obtained by suction filtration. The solid is washed with water and dried to obtain white carbon black. The filtrate was distilled out of all the trimethylamine in the system under a pressure of 0.2 bar at a temperature of 80°C, and then the temperature of the system was maintained at the same pressure, and the temperature was increased to 120°C to obtain HF.

Embodiment 3

[0035] Mix 50 g of a 20% fluorosilicic acid solution and 80 g of tri-n-octylamine, gradually increase the temperature to 60 ℃, and mix and stir for 1.5 h. Then, the water phase was separated by liquid separation, 36 g of trimethylamine was added to the organic phase, and the reaction was carried out for 1.5 h, and the solid and the filtrate were obtained by suction filtration. The solid is washed with water and dried to obtain white carbon black. The filtrate was steamed out of the system at a temperature of 90°C under normal pressure, and then the temperature and pressure of the system remained unchanged, and the temperature was increased to 120°C to obtain HF.

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Abstract

The invention particularly relates to a method for preparing hydrogen fluoride (HF) and white carbon black by treating fluosilicic acid (H2SiF6) via an organic alkali, which relates to the technical field of chemical engineering. The method comprises the following steps: a, extracting a H2SiF6 solution with an extractant; b, adding the organic alkali with a low boiling point into a H2SiF6-extractant solution to perform a reaction on the organic alkali and the H2SiF6 so as to generate SiO2 and an organic alkali fluoride salt which are filtered, thereby obtaining the white carbon black; c, heating the organic alkali fluoride salt to a certain temperature and distilling so as to remove the organic alkali with the low boiling point, thereby obtaining a HF-extractant solution; and d, heating, distilling and separating the HF-extractant solution so as to obtain the HF product and recycling the extractant after the regeneration of the extractant so as to extract the H2SiF6. According to the method, fluorine and silicon resources in byproducts in the phosphate fertilizer industry are efficiently and comprehensively utilized.

Description

technical field [0001] The invention relates to a method for preparing hydrogen fluoride and white carbon black by treating a fluorosilicic acid solution with an organic base, in particular to a method for efficiently utilizing by-product dilute fluorosilicic acid resources in the production process of wet-process phosphoric acid and phosphate fertilizer. It belongs to the field of chemical technology. Background technique [0002] Hydrogen fluoride is the basis of modern fluorine chemical industry and the most basic raw material for producing various fluorine products, and the market demand is huge. At present, almost all the fluorine in the fluorine chemical industry comes from the mining of fluorite, but as a non-renewable resource, the excessive consumption of fluorite in recent years has attracted the attention of all parties. As the country controls and reduces the production of fluorite, it will inevitably lead to a shortage of raw materials for fluorine chemical com...

Claims

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Application Information

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IPC IPC(8): C01B33/113C01B7/19
Inventor 黄忠杜璐杉田强李玉叶
Owner 云天化集团有限责任公司