Calcium Fluoride Production from Concentrated Fluosilicic Acid

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current processes for producing calcium fluoride from fluosilicic acid suffer from impurities, long reaction times, and limitations in using concentrated fluosilicic acid, making them unsuitable for industrial applications, particularly in hydrogen fluoride production and fluorine reserve storage.

Innovation Solution

A process involving the reaction of fluosilicic acid with ammonium hydroxide to form a slurry, followed by precipitation with calcium carbonate, allowing for the production of high-grade synthetic calcium fluoride and active silica, with ammonia recycling to enhance efficiency and purity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If diluted fluosilicic acid (2.5-3.8% concentration) is reacted with lime to produce calcium fluoride, then the reaction can be carried out in a controlled pH range (3.5-6.7), but the calcium fluoride product contains 4-7% SiO2 impurity which reduces its suitability for hydrogen fluoride production

Engineering Contradiction:
Improvereaction controlVSAvoidproduct purity
Core Design Contradiction:
ReliabilityVSManufacturing precision

Solution Approach 1:

The patent changes the concentration parameter of fluosilicic acid from the conventional diluted range (2.5-3.8%) to a concentrated range (20-40%), and adjusts the pH range to 4.0-6.0. This parameter change enables the use of concentrated acid while maintaining reaction control and achieving high purity calcium fluoride product with less than 0.5% SiO2 impurity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent follows the proven reaction mechanism and pH control approach from U.S. Pat. No. 2,780,521 but modifies the concentration parameters to achieve both reaction control and high product purity simultaneously, effectively creating an improved version of the conventional process

Inventive Principle:
Principle #26Copying

2Productivity

If concentrated fluosilicic acid (20-40% concentration) is used in the reaction with lime, then the productivity and efficiency improve, but the reaction becomes difficult to control and requires special conditions

Engineering Contradiction:
Improveproduction efficiencyVSAvoidreaction controllability
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The patent establishes specific parameter ranges: fluosilicic acid concentration of 20-40%, pH range of 4.0-6.0, and temperature of 20-50°C. These parameter changes enable the use of concentrated acid for high productivity while maintaining reaction controllability through defined operational boundaries

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent implements dynamic pH control during the reaction process to maintain the pH within the 4.0-6.0 range, allowing the reaction to proceed efficiently with concentrated acid while preventing unwanted side reactions and ensuring consistent product quality

Inventive Principle:
Principle #15Dynamics

3Ease of manufacture

If the conventional neutralization process with lime is used, then the process is simple, but the calcium fluoride product has high SiO2 content (4-7%) that limits its industrial applications

Engineering Contradiction:
Improveprocess simplicityVSAvoidproduct purity
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent maintains the simplicity of the lime neutralization process but changes the concentration parameters: using concentrated fluosilicic acid (20-40%) instead of diluted acid, and controlling pH in the 4.0-6.0 range. These changes produce high purity calcium fluoride with less than 0.5% SiO2 while keeping the process straightforward and industrially viable

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This process achieves high-grade calcium fluoride (>90% CaF2) and active silica production, suitable for hydrogen fluoride production and other industrial uses, while minimizing costs and overcoming previous process limitations.

Implementation Method 1

reacting fluosilicic acid with ammonium hydroxide or ammonia in a first reactor so as to obtain a first slurry

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

filtering said first slurry so as to obtain a filtrate containing a solution of ammonium fluoride

Methodology Applied
Scientific EffectFiltration: Filter (physical)

Implementation Method 3

precipitating the solution of ammonium fluoride obtained as a filtrate in step (a) with calcium carbonate as a dry form or as a suspension in a second reactor so as to produce a second slurry containing calcium fluoride

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 4

filtering said second slurry so as to obtain a filter cake containing calcium fluoride and a filtrate containing a solution of ammonium carbonate

Methodology Applied
Scientific EffectFiltration: Filter (physical)

Implementation Method 5

drying said filter cake so as to obtain calcium fluoride and a filter cake washing containing a solution of ammonium carbonate

Methodology Applied
Scientific EffectEvaporation: Evaporation

Data Source

PatentUS11873229B2Process for preparing calcium fluoride from fluosilicic acid
Publication Date: 2024.01.16 OCP SA
  • US11873229B2 patent drawing

AI summary

A process for preparing synthetic calcium fluoride (CaF2) (min 90% CaF2 by weight) from fluosilicic acid is provided. The processes comprises the steps of (a) reacting fluosilicic acid (H2SiF6) with ammonium hydroxide or ammonia in a first reactor so as to obtain a first slurry and filtering the first slurry so as to obtain a filtrate containing a solution of ammonium fluoride (b) precipitating the solution of ammonium fluoride with calcium in a second reactor so as to produce a second slurry containing calcium fluoride and (c) evolving the major part of ammonia from the second reactor and then scrubbing and returning said ammonia to the first reactor.