US 11,891,344 B2
Methods for graded utilization of fluorine and silicon resources in phosphate ores
Xiaowei Quan, Guiyang (CN)
Assigned to CHTEM LIMITED, Guiyang (CN)
Filed by CHTEM LIMITED, Guizhou (CN)
Filed on Apr. 5, 2023, as Appl. No. 18/296,356.
Application 18/296,356 is a continuation of application No. PCT/CN2023/081412, filed on Mar. 14, 2023.
Claims priority of application No. 202210413670.0 (CN), filed on Apr. 20, 2022.
Prior Publication US 2023/0339822 A1, Oct. 26, 2023
Int. Cl. C05B 11/08 (2006.01); C01B 7/19 (2006.01); C01B 33/107 (2006.01)
CPC C05B 11/08 (2013.01) [C01B 7/196 (2013.01); C01B 33/10705 (2013.01)] 19 Claims
OG exemplary drawing
 
1. A method for a graded utilization of fluorine and silicon resources in a phosphate ore, comprising:
Step (1), acidification: mixing sulfuric acid or phosphoric acid with the phosphate ore for reacting to produce dilute phosphoric acid or phosphate fertilizer while generating tail gas including fluorine and silicon;
Step (2), absorption: obtaining an acidic solution including fluorine and silicon by absorbing the tail gas with water;
Step (3), osmosis thickening: obtaining a dilute solution by performing an osmosis operation on the acidic solution using a driving solution, wherein the driving solution absorbs part of solvent of the acidic solution to obtain the dilute solution; and the acidic solution increases in concentration to obtain a concentrated solution; and the osmosis operation is a forward osmosis, wherein the driving solution is a phosphate solution or a phosphoric acid solution, and the dilute solution includes a dilute phosphate solution or a dilute phosphoric acid solution;
Step (4), concentration and filtration: performing a concentration operation by passing silicon fluoride gas into the concentrated solution to continuously increase concentration of the concentrated solution; and filtering and separating the concentrated solution to obtain silicon dioxide (SiO2), a fluorine-containing solution, and waste gas;
Step (5), extraction: obtaining a loaded phase and a raffinate by adding an extract phase to the fluorine-containing solution, mixing and extracting thoroughly, and separating phases;
Step (6), liquid adsorption: obtaining a refined solution by adsorbing and removing impurities from the raffinate;
Step (7), dehydration: obtaining crude silicon tetrafluoride (SiF4) and an HF-sulfuric acid (H2504) solution by adding a dehydrant to the refined solution and mixing thoroughly, and producing anhydrous hydrogen fluoride with a purity of not less than 99% and waste sulfuric acid as a by-product by performing steam stripping and distillation on the separate HF—H2SO4 solution;
Step (8), decontamination: obtaining decontamination gas by adsorbing impurities in the crude SiF4 by gaseous adsorption; and
Step (9), low-temperature distillation: obtaining impurity gas, and SiF4 with a purity of not less than 99% by performing a low-temperature distillation on the decontamination gas to remove impurities with low and high boiling points.