Method for aminolysis of fluorosilicone compounds and separation of fluorine and silicon

A separation method and compound technology, applied in the field of ammonolysis and separation of fluorine and silicon elements, can solve the problems of low conversion rate, low concentration of ammonium fluoride, and deterioration of technical and economic indicators, so as to reduce content, increase conversion rate and improve The effect of techno-economic indicators

Inactive Publication Date: 2006-12-27
GUIYANG KAILIN FERTILIZER CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ammonolysis and fluorine-silicon element separation methods of these technologies have the following defects: ①NH 4 F conversion rate is low: depending on the NH in the solution 4 Depending on the concentration of F and the reaction temperature, the conversion rate is only 70% to 95%; ②The ammonium fluoride solution contains a large amount of unprecipitated silica, which exists in the form of ammonium fluorosilicate, and contains NH 4 F SiO in 20%~45% ammonium fluo

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: 50 g of solid ammonium fluorosilicate with a content of 98% was added to 250 g of saturated ammonium fluoride circulating reaction liquid, and 20 g of raw material gas ammonia was introduced simultaneously to carry out the ammonolysis reaction. Saturated ammonium fluoride circulating reaction solution NH 4 The F content is 47%, the temperature is 30°C, and three cycles have been passed. After the temperature reached 60° C., the reaction slurry was cooled down, and the reaction was continued by feeding. After 60 minutes of adding the raw materials and the temperature of the slurry dropped to 30°C, the reaction slurry was screened with a 325-mesh screen to obtain ammonium fluoride crystal slurry and silicon dioxide suspension. Silica suspension was filtered to obtain silica filter cake and saturated ammonium fluoride solution. The silica filter cake was washed and burned to obtain 16.3 g of silica. The resulting ammonium fluoride crystal slurry was filtered ...

Embodiment 2

[0020] Example 2: SiF4 gas was passed into 300 g of saturated ammonium fluoride circulating reaction solution, and 40 g of raw material gas ammonia was passed through at the same time to carry out ammonolysis reaction. Silicon tetrafluoride gas SiF 4 Net content is 52g, concentration is 33%; saturated ammonium fluoride circulating reaction solution NH 4 The F content is 45%, the temperature is 20°C, and the second cycle has been passed. After the temperature reaches 50°C, the reaction slurry is cooled and the reaction is continued by feeding. After 90 minutes of adding the raw materials and the temperature of the slurry dropped to 20°C, the reaction slurry was screened with a 400-mesh screen to obtain ammonium fluoride crystal slurry and silica suspension. Silica suspension was filtered to obtain silica filter cake and saturated ammonium fluoride solution. The silica filter cake was washed and burned to obtain 29.5 g of silica. The resulting ammonium fluoride crystal slurr...

Embodiment 3

[0021] Embodiment 3: the ammonium fluorosilicate filter cake that 50g content is 98% is added in 350g saturated ammonium fluoride circulating reaction liquid, feeds raw material gas ammonia 22g simultaneously and carries out ammonolysis reaction; Saturated ammonium fluoride circulating reaction liquid NH 4 The F content is 42.5%, the temperature is 10°C, and one cycle has been passed. After the temperature reaches 80°C, the reaction slurry is cooled and the reaction is continued by feeding. After 100 minutes of adding the raw materials and the temperature of the slurry dropped to 10°C, the reaction slurry was screened with a 325-mesh screen to obtain ammonium fluoride crystal slurry and silica suspension. Silica suspension was filtered to obtain silica filter cake and saturated ammonium fluoride solution. The silica filter cake was washed and burned to obtain 16.5 g of silica. The resulting ammonium fluoride crystal slurry was filtered to obtain 72 g of high-content wet ammo...

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PUM

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Abstract

The invention discloses a separating method of aminolysis and hydrofluosilicic element of silicofluoride, which comprises the following steps: 1. adding solid ammonium fluosilicate or silicon tetrafluoride gas in the saturated ammonium fluoride circulating reacting liquid; putting raw material amino to proceed aminolysis reaction; 2. reducing slurry temperature; screening the reacted slurry; 3. filtering the screened silica suspension and ammonium fluoride crystal slurry to obtain saturated ammonium fluoride solution, silica solid and ammonium fluoride crystal; returning to former procedures as the circulating reacting liquid; washing the ammonium fluoride crystal; drying through normal drying method to obtain high-purity product. The invention can improves technological and economical index, which is fit for wet-producing phosphoric acid, phosphate fertilizer and other phosphor businesses.

Description

technical field [0001] The invention relates to inorganic fluorosilicon compounds such as silicon tetrafluoride, fluorosilicic acid, and fluorosilicate produced during the processing of wet-process phosphoric acid and phosphate fertilizer, in particular to the ammonolysis of fluorosilicon compounds and the separation method of fluorosilicon elements. Background technique [0002] It is well known that inorganic fluorosilicon compounds such as silicon tetrafluoride, fluorosilicic acid and fluorosilicate will be produced during the processing of wet-process phosphoric acid and phosphate fertilizer. If these by-products are not recycled, they will not only pollute the environment, but also cause waste of resources. The inorganic fluorosilicon compound is converted into ammonium fluoride and silicon dioxide by reacting with ammonia, ammonium hydroxide or ammonium carbonate, and then the ammonium fluoride and silicon dioxide are separated by filtration, thereby realizing the separ...

Claims

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Application Information

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IPC IPC(8): C01C1/16C01B33/08
Inventor 朱建国唐波张筑楠陈文兴丁禹
Owner GUIYANG KAILIN FERTILIZER CO LTD
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