Method for producing hydrogen fluoride

Patent metadata

Field	Value
Publication number	US-11718523-B2
Application number	US-202117159844-A
Country	US
Kind code	B2
Filing date	Jan 27, 2021
Priority date	Jul 11, 2014
Publication date	Aug 8, 2023
Grant date	Aug 8, 2023

Abstract

The present invention provides a novel method for producing hydrogen fluoride which can suppress the occurrence of the pasty state over the whole process of producing hydrogen fluoride, reduce the problem of corrosion caused by sulfuric acid, and improve energy efficiency of the process. A method for producing hydrogen fluoride by reacting calcium fluoride and sulfuric acid comprises: (a) mixing and reacting calcium fluoride and sulfuric acid such that a mixture comprising calcium fluoride particles and sulfuric acid substantially maintains a form of particulate to obtain hydrogen fluoride while supplying sulfuric acid to the calcium fluoride particles at a flow rate of 0.002 to 1 mol/min relative to 1 mol of calcium fluoride to such an amount that a molar ratio of sulfuric acid/calcium fluoride is 0.9 to 1.1.

First claim

The invention claimed is:

1. A method for producing hydrogen fluoride by reacting calcium fluoride and sulfuric acid, the method comprising:
(a) mixing and reacting calcium fluoride and sulfuric acid such that a mixture comprising calcium fluoride particles and sulfuric acid substantially maintains a particulate form to obtain hydrogen fluoride while supplying sulfuric acid to the calcium fluoride particles at a flow rate of 0.002 to 0.07 mol/min relative to 1 mol of calcium fluoride to such an amount that a molar ratio of sulfuric acid/calcium fluoride is 0.9 to 1.1,
wherein the mixing in step (a) is continued after finishing the supply of sulfuric acid until the reaction between calcium fluoride and sulfuric acid is completed.

2. The method according to claim 1 , wherein the mixing is conducted in the step (a) by use of an apparatus having an attainment degree of mixing of 0.1 or more one minute after a start of the mixing.

3. The method according to claim 1 , wherein the step (a) is conducted at a temperature of 0 to 500° C.

4. The method according to claim 1 , wherein the calcium fluoride particles have a specific surface area of 0.5 to 30 m 2 /g.

5. The method according to claim 1 , wherein the particulate form in which the mixture comprising calcium fluoride particles and sulfuric acid is substantially maintained is confirmed during the mixing by at least one of:
(i) observation of rapid rise and/or hunting in a torque and/or a current value of a stirring machine used for the mixing, and
(ii) comparison of a theoretical value of an amount of generated hydrogen fluoride which is calculated based on the amount of sulfuric acid applied at one time point in the step (a), with the amount of hydrogen fluoride generated at the one time point.

6. The method according to claim 1 , wherein the confirmation of at least one of the (i) observation and (ii) comparison is conducted in combination with (iii) visual observation.

Assignees

• Daikin Ind Ltd

Inventors

• Sasatani Arata
• Kinoshita Toshiyuki
• Yoshimura Toshikazu
• Tabuchi Akikazu
• Imoto Masayoshi

Classifications

• C01B7/191 Primary

  Hydrogen fluoride · CPC title

• C01B7/192 Primary

  Preparation from fluorspar · CPC title

• C01B9/08

  Fluorides · CPC title

• C01B7/19 Primary

  Fluorine; Hydrogen fluoride · CPC title

• C01B17/69

  Sulfur trioxide; Sulfuric acid · CPC title