Automated production method for producing fluorine-containing crystalline products using fluorine-containing solutions

Abstract

This invention provides an automated production method for producing fluorine-containing crystalline products using a fluorine-containing solution, comprising: treating the fluorine-containing solution with a nanofiltration membrane to obtain a treated solution, and presetting a first feed amount; feeding the treated solution into a reagent mixing tank; providing a reaction solution with a predetermined concentration; sensing the molar concentration of fluoride ions and the molar concentration of ammonium ions in the treated solution; an automatic control module outputting a second feed amount based on the first feed amount of the treated solution, the molar concentrations of fluoride ions and ammonium ions, and the predetermined concentration of the reaction solution, and feeding the reaction solution of the second feed amount into the reagent mixing tank to form a mixing solution; sending the mixing solution into a concentration tower to concentrate the mixing solution to obtain a concentrated solution; and subjecting the concentrated solution to a crystallization reaction to obtain a fluorine-containing crystalline product.

Claims

1. An automated production method for producing fluorine-containing crystalline products using a fluorine-containing solution, comprising: A fluorinated solution is provided, which contains hydrofluoric acid, ammonium fluoride, or a combination thereof; The fluoride-containing solution is treated with a nanofiltration membrane to obtain a treated solution, and a first feed amount of the treated solution is preset; the treated solution is fed into a reagent mixing tank at the first feed amount; A reaction solution with a predetermined concentration is provided, which is a hydrofluoric acid solution or an ammonia solution; the concentrations of fluoride ions and ammonium ions in the treatment solution in the reagent mixing tank are sensed; an automatic control module outputs a second feed amount of the reaction solution based on the first feed amount of the treatment solution, the concentrations of fluoride ions and ammonium ions, and the predetermined concentration of the reaction solution, and feeds the second feed amount of the reaction solution into the reagent mixing tank to form a mixing solution; The prepared solution is fed into a concentration tower for concentration, and the molar concentrations of fluoride ions and ammonium ions in the concentration tower are sensed. Based on these molar concentrations, the automatic control module outputs a third feed rate for the reaction solution. This third feed rate of the reaction solution is then fed into the concentration tower to obtain a concentrated solution with a specific gravity of 1.1 to 1.

3. The concentrated solution is subjected to a crystallization reaction to obtain a fluorinated crystalline product, which is either an ammonium fluoride crystalline product or an ammonium bifluoride crystalline product. When the fluorinated crystalline product is an ammonium fluoride crystalline product, if the ratio of the fluoride molar concentration to the ammonium ion molar concentration in the treated solution is less than 0.95, the reaction solution fed into the reagent mixing tank is a hydrofluoric acid solution. If the ratio of the fluoride molar concentration to the ammonium ion molar concentration in the treated solution is greater than 1.00, the reaction solution fed into the reagent mixing tank is an ammonia solution. If the ratio of the fluoride molar concentration to the ammonium ion molar concentration in the mixed solution in the concentration tower is less than 0.95, the reaction solution fed into the concentration tower is a hydrofluoric acid solution. If the ratio of the fluoride molar concentration to the ammonium ion molar concentration in the mixed solution in the concentration tower is greater than 1.00, the reaction solution fed into the concentration tower is an ammonia solution. Specifically, when the fluorine-containing crystalline product is an ammonium bifluoride crystalline product, if the ratio of the molar concentration of fluoride ions to the molar concentration of ammonium ions in the treatment solution is less than 2.00, the reaction solution fed into the reagent mixing tank is the hydrofluoric acid solution; if the ratio of the molar concentration of fluoride ions to the molar concentration of ammonium ions in the treatment solution is greater than 2.05, the reaction solution fed into the reagent mixing tank is the ammonia solution; if the ratio of the molar concentration of fluoride ions to the molar concentration of ammonium ions in the mixing solution in the concentration tower is less than 2.00, the reaction solution fed into the concentration tower is the hydrofluoric acid solution; if the ratio of the molar concentration of fluoride ions to the molar concentration of ammonium ions in the mixing solution in the concentration tower is greater than 2.05, the reaction solution fed into the concentration tower is the ammonia solution.

2. The automated production method as described in claim 1, wherein between the aforementioned step of feeding the second amount of the reaction solution into the reagent mixing tank and the aforementioned step of feeding the mixing solution into the concentration tower to concentrate the mixing solution, the automated production method includes: When the fluorinated crystalline product is an ammonium fluoride crystalline product and the ratio of the fluoride ion mole concentration to the ammonium ion mole concentration of the prepared solution is sensed to be 0.95 to 1.0, or when the fluorinated crystalline product is an ammonium bifluoride crystalline product and the ratio of the fluoride ion mole concentration to the ammonium ion mole concentration of the prepared solution is sensed to be 2.0 to 2.05, the prepared solution is sent into a storage tank.

3. The automated production method as described in claim 1, wherein the step of treating the fluoride-containing solution using the nanofiltration membrane includes: The fluorine-containing solution is treated at a temperature of 20°C to 40°C and a pressure of 0.5 MPa to 1.5 MPa to obtain the treated solution.

4. The automated production method as described in claim 1, wherein the pore size of the nanofiltration membrane is from 0.2 nanometers to 1.8 nanometers.

5. The automated production method as described in claim 1, wherein the step of treating the fluoride-containing solution using the nanofiltration membrane includes: The fluoride-containing solution is treated with a filter, and then treated with a nanofiltration membrane to obtain the treated solution.

6. The automated production method as described in claim 5, wherein the filter comprises a polypropylene filter membrane having a pore size of 1.0 micrometer to 10.0 micrometer.

7. The automated production method as described in claim 1, wherein the step of concentrating the prepared solution includes: The prepared solution was concentrated at a temperature of 30°C to 80°C and a vacuum of -30 cmHg to -80 cmHg to obtain the concentrated solution.

8. The automated production method as described in claim 1, wherein the step of causing the concentrated solution to undergo a crystallization reaction includes: The concentrated solution was subjected to a crystallization reaction at a temperature between 2°C and 25°C.

9. The automated production method as described in any one of claims 1 to 8, wherein the purity of the fluorine-containing crystalline product is 95% or higher.

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