Method for preparing high-purity carbon oxysulfide gas

Abstract

The invention discloses a method for preparing high-purity carbon oxysulfide gas. The method comprises the following steps of: (i) synthetic reaction: allowing saturated ammonium thiocyanate solution to react with sulfuric acid in a reactor to generate the carbon oxysulfide gas containing impurities; (ii) alkaline washing: continuously introducing the carbon oxysulfide gas containing impurities into a primary alkaline washing tower and a secondary washing tower to remove trace acidic impurities; (iii) primary drying; (vi) secondary drying; and (v) rectification. The method has the advantages of simple equipment, convenience of operation, safe equipment operation, high yield and the like.

Description

technical field

[0001] The invention belongs to a method for preparing carbon oxysulfide gas, in particular to a method for preparing high-purity carbon oxysulfide gas by using sulfuric acid and ammonium thiocyanate as raw materials. Background technique

[0002] Carbonyl sulfide, also known as carbonyl sulfide or carbonyl sulfide, is an important raw material for the synthesis of thiocarbamate pesticides and insecticides, and an important pharmaceutical intermediate and food fumigant.

[0003] In recent years, high-purity carbon oxysulfide has been found to have special effects in the etching process of integrated circuits. The world's leading integrated circuit manufacturer has established a chip etching production line using carbon oxysulfide as raw material, and the process has Trend spreading to all IC manufacturers.

[0004] There are many methods for preparing carbon oxysulfide gas, and the commonly used methods for preparing carbon oxysulfide gas include dry synthes...

Examples

Embodiment 1

[0058] Add an appropriate amount of sulfuric acid with a concentration of 50% into the reactor 2, and heat the reactor to 70°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 70 and 80°C. The reactant is carbon oxysulfide gas containing impurities.

[0059] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0060]The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washing...

Embodiment 2

[0066] Add an appropriate amount of sulfuric acid with a concentration of 65% into the reactor 2, and heat the reactor to 50°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 50 and 60°C. The reactant is carbon oxysulfide gas containing impurities.

[0067] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0068] The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washin...

Embodiment 3

[0074] Add an appropriate amount of sulfuric acid with a concentration of 80% into the reactor 2, and heat the reactor to 30°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 30 and 40°C. The reactant is carbon oxysulfide gas containing impurities.

[0075] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0076] The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washin...

technical field

[0001] The invention belongs to a method for preparing carbon oxysulfide gas, in particular to a method for preparing high-purity carbon oxysulfide gas by using sulfuric acid and ammonium thiocyanate as raw materials. Background technique

[0002] Carbonyl sulfide, also known as carbonyl sulfide or carbonyl sulfide, is an important raw material for the synthesis of thiocarbamate pesticides and insecticides, and an important pharmaceutical intermediate and food fumigant.

[0003] In recent years, high-purity carbon oxysulfide has been found to have special effects in the etching process of integrated circuits. The world's leading integrated circuit manufacturer has established a chip etching production line using carbon oxysulfide as raw material, and the process has Trend spreading to all IC manufacturers.

[0004] There are many methods for preparing carbon oxysulfide gas, and the commonly used methods for preparing carbon oxysulfide gas include dry synthes...

Examples

Embodiment 1

[0058] Add an appropriate amount of sulfuric acid with a concentration of 50% into the reactor 2, and heat the reactor to 70°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 70 and 80°C. The reactant is carbon oxysulfide gas containing impurities.

[0059] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0060]The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washing...

Embodiment 2

[0066] Add an appropriate amount of sulfuric acid with a concentration of 65% into the reactor 2, and heat the reactor to 50°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 50 and 60°C. The reactant is carbon oxysulfide gas containing impurities.

[0067] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0068] The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washin...

Embodiment 3

[0074] Add an appropriate amount of sulfuric acid with a concentration of 80% into the reactor 2, and heat the reactor to 30°C after evacuating the reactor 2 to test for leaks. Add the saturated solution prepared with 15 kilograms of ammonium thiocyanate in raw material tank 1. Open the reactor inlet valve 4 and the ammonium thiocyanate saturated solution enters the reactor through the pipeline 3 and starts to react with sulfuric acid. Between 30 and 40°C. The reactant is carbon oxysulfide gas containing impurities.

[0075] Analyzing the reactor to analyze the gas composition at the outlet of the reactor, the gas contains a small amount of oxygen (O 2 ), nitrogen (N 2 ) carbon dioxide (CO 2 ), carbon monoxide (CO), carbon disulfide (CS 2 ), hydrogen sulfide (H 2 S), water (H 2 O), and carbon oxysulfide (COS) gas.

[0076] The carbon oxysulfide gas that contains impurity enters alkali washing tower 6 and alkali washing tower 7 continuously and carries out alkali washin...

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