Preparation method for anhydrous hydrogen fluoride

A technology of anhydrous hydrogen fluoride and hydrogen fluoride gas, applied in the direction of fluorine/hydrogen fluoride, etc., can solve problems such as long reaction time, achieve the effects of improving utilization rate, reducing the amount of sulfuric acid, and saving heat energy

Active Publication Date: 2014-06-11
FUJIAN YONGJING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this invention still cannot completely avoid the occurrence of "back-mix

Method used

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  • Preparation method for anhydrous hydrogen fluoride
  • Preparation method for anhydrous hydrogen fluoride
  • Preparation method for anhydrous hydrogen fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] a) Pre-reaction

[0069] a-1) Mix concentrated sulfuric acid and fuming sulfuric acid according to the weight ratio of 1:1.43 and send it to the mixed acid heater. The heating time is 7 minutes and the heating temperature is 110°C;

[0070] a-2) Send the fluorspar powder into the powder drying furnace, and use the residual gas heated by the external jacketed converter for heating, the heating time is 75 minutes, and the heating temperature is 175°C;

[0071] a-3) Put the heated mixed sulfuric acid and fluorspar powder into the pre-reactor for mixing according to the weight ratio of 1:1.25 to obtain the mixed material. The mixing temperature is 120°C and the mixing time is 12 minutes. The crude hydrogen fluoride gas produced after mixing accounts for 6% of the total, and enters the converter reactor together with the heated mixed material.

[0072] b) Reaction:

[0073] The heated mixed material is continuously fed into the converter reactor, and the reaction is carrie...

Embodiment 2

[0086] a) Pre-reaction

[0087] a-1) Mix concentrated sulfuric acid and fuming sulfuric acid according to the weight ratio of 1:1.45 and send it to the mixed acid heater, the heating time is 8 minutes, and the heating temperature is 100°C;

[0088] a-2) Send the fluorspar powder into the powder drying furnace, and use the residual gas heated by the external jacketed converter for heating, the heating time is 80 minutes, and the heating temperature is 180°C;

[0089] a-3) Put the heated mixed sulfuric acid and fluorspar powder into the pre-reactor for mixing according to the feeding weight ratio of 1:1.20 to obtain the mixed material. The mixing temperature is 100°C and the mixing time is 15 minutes. The crude hydrogen fluoride gas produced after mixing accounts for 4% of the total, and enters the converter reactor together with the mixed materials.

[0090] b) Reaction:

[0091] In the reaction stage, the temperature in the converter is controlled as front temperature: 550°C...

Embodiment 3

[0100] a) Pre-reaction

[0101] In the pre-reaction stage, except that the weight ratio of concentrated sulfuric acid and oleum is 1:1.40, the heating time is 7 minutes, the heating temperature is 120°C, the heating time of fluorspar powder is 90 minutes, and the heating temperature is 150°C, mixed sulfuric acid and fluorspar powder The weight ratio of the feedstock was 1:1.29, the mixing temperature was 150° C., and the mixing time was 10 minutes. The crude hydrogen fluoride gas generated after mixing accounted for 5% of the total amount, and the rest were the same as in Example 1.

[0102] b) Reaction:

[0103] In the reaction stage, the temperature in the converter is controlled as front temperature: 650°C, middle temperature: 700°C, middle and back temperature: 720°C, back temperature: 750°C, the speed of the converter reactor is 2r / min, and the pressure in the converter is -0.45 KPa, the reaction times is 50 minutes, and the weight ratio of returning material is except t...

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Abstract

A disclosed preparation method for anhydrous hydrogen fluoride comprises the following steps: respectively adding a mixed sulfuric acid ( concentrated sulfuric acid and oleum) and fluorspar powder according to a certain material pouring ratio into a pre-reactor for a pre-reaction; sending to a converter reactor, reacting under the heating condition to obtain a large amount of crude hydrogen fluoride gas; and processing by a washing tower, a condenser, a rectifying tower and a degassing tower, so as to prepare pure hydrogen fluoride gas. An incompletely reacted material in the converter reactor is processed through recycle, and a gas uncollected after the crude hydrogen fluoride gas generated in the reaction is refined is secondarily utilizable through two-time circulation absorption, so that the yield of the preparation method is substantially improved.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a preparation method of anhydrous hydrogen fluoride. Background technique [0002] Anhydrous hydrogen fluoride is widely used in atomic energy, chemical industry, petroleum and other industries. It is a strong oxidant and can be used to prepare elemental fluorine, various fluorine refrigerants, inorganic fluorides, organic fluorides, and can also be formulated into aqueous hydrogen for various purposes. Hydrofluoric acid. The traditional preparation method of anhydrous hydrogen fluoride is mainly to mix fluorspar powder and sulfuric acid, and directly produce hydrogen fluoride under heating conditions. [0003] The main chemical reactions are: [0004] CaF 2 (s)+H 2 SO 4 (l) → CaSO 4 (s)+2HF (g) (1) [0005] The main side effects are: [0006] SiO 2 +4HF→SiF 4 +H 2 O→SiF 4 (2) [0007] SiF 4 +2HF→H 2 SiF 6 ...

Claims

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Application Information

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IPC IPC(8): C01B7/19
Inventor 吴云秀饶仁
Owner FUJIAN YONGJING TECH CO LTD
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