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Preparation method and preparation apparatus of carbonyl sulfide

A carbonyl sulfide and elemental sulfur technology, applied in the directions of carbon oxysulfide, carbon sulfur compounds, etc., can solve the problems of difficulty in ensuring the quality stability of carbonyl sulfide, difficult to obtain high-purity carbonyl sulfide products, and unsuitable for mass preparation, etc. It is easy to achieve large-scale industrial production, reasonable process steps and equipment, and suitable catalyst selection.

Pending Publication Date: 2019-01-18
欧中汇智电子材料研究院(重庆)有限公司
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Problems solved by technology

Among them, the carbon monoxide method is divided into solvent-free and solvent-free. The process is relatively simple and the yield is high. Considering the cost and source of raw materials, this process is generally used in industrial production, but the reaction speed is slow and there are more impurities. Such as hydrogen sulfide, sulfur dioxide, carbon dioxide, etc., which affect the purity of the product
The urea method, potassium thiocyanate method, ammonium thiocyanate method and other processes have the characteristics of small and exquisite synthesis equipment and easy operation. However, due to the existence of solvent water, it is easy to further decompose the product carbon oxysulfide into impurities, increasing the purification efficiency. Difficulty, and the waste water produced by this method is difficult to treat, so it is not suitable for mass production
[0004] In general, in the existing above-mentioned carbonyl sulfide synthesis process, the reaction rate is relatively slow, and more impurities will be produced while making carbonyl sulfide, wherein SO 2 、H 2 S, CO 2 The boiling point of carbonyl sulfide is relatively close, and both are acid gases, which are not easy to remove
Carbonyl sulfide also has a characteristic that it is easy to hydrolyze to generate H 2 S and CO 2 , if the water content is high, it is difficult to ensure the stability of carbonyl sulfide quality
Therefore, it is difficult to produce high-purity carbonyl sulfide products that meet market needs in industrial production

Method used

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  • Preparation method and preparation apparatus of carbonyl sulfide

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preparation example Construction

[0055] In a first aspect, a method for preparing carbonyl sulfide is provided in at least one embodiment, comprising the steps of:

[0056] Pass carbon monoxide and elemental sulfur vapor into a reactor equipped with a metal sulfide catalyst to carry out a synthesis reaction to obtain a mixed gas; the mixed gas is a mixed gas containing carbonyl sulfide;

[0057] After the mixed gas is separated, unreacted elemental sulfur vapor, unreacted carbon monoxide and carbonyl sulfide are obtained, and the unreacted elemental sulfur vapor and unreacted carbon monoxide are returned to the reactor for cyclic reaction;

[0058] The carbonyl sulfide is condensed and collected in a low-temperature collection tank, and then enters a purification system for purification to obtain high-purity carbonyl sulfide.

[0059] The invention uses carbon monoxide and elemental sulfur (sulfur powder) as raw materials for preparation, reacts to synthesize crude products under the action of metal sulfide c...

Embodiment approach

[0099] As a preferred embodiment of the present invention, the process of the process includes:

[0100] a). The metal sulfide catalyst is loaded into the reactor and distributed evenly;

[0101] b). Feed carbon monoxide and elemental sulfur vapor into the reactor under suitable temperature and pressure conditions for reaction, and the mixed gas discharged after the reaction contains unreacted carbon monoxide and elemental sulfur vapor, as well as generated carbonyl sulfide gas;

[0102] c). Pass the mixed gas discharged from the reactor into the gas-solid separator, intercept the unreacted elemental sulfur vapor, and then pass it into the low-temperature collection tank to collect the crude product of carbonyl sulfide, and the raw material carbon monoxide that has not been condensed After being pressurized by the compressor, it returns to the middle reactor to carry out the reaction again;

[0103] d). The amount of carbon monoxide added can be determined according to the pr...

Embodiment 1

[0127] Such as figure 1 As shown, this embodiment provides a carbonyl sulfide preparation device, including a carbon monoxide raw material supply system, an elemental sulfur raw material supply system, a reactor 3, a separation device, a low-temperature collection tank 5 and a purification system;

[0128] Wherein, the metal sulfide catalyst is filled in the reactor 3; the metal sulfide comprises BaS, FeS, FeS 2 or CaSO 4 at least one of them; the loading volume of the metal sulfide is 2 / 3 to 4 / 5 of the volume of the reactor 3; the material of the reactor 3 includes at least one of monel, inconel and acid-resistant nickel alloy kind.

[0129] The separation device includes a gas-solid separator 4; the purification system includes an adsorption dryer 6 and a rectification device; the adsorbent in the adsorption dryer 6 includes 3A molecular sieves and / or mordenite molecular sieves; the rectification device includes at least two series-connected The rectification tower 7 and ...

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Abstract

The invention belongs to the technical field of industrial gas preparation, and relates to a preparation method and preparation apparatus of carbonyl sulfide. The preparation method of the carbonyl sulfide comprises the following steps: introducing carbon oxide and element sulfur steam into a reactor with a metal sulfide catalyst, and performing the synthetic reaction, thus obtaining mixed gas; separating the mixed gas, thus obtaining the unreacted element sulfur steam, unreacted carbon oxide and carbonyl sulfide, and returning the unreacted element sulfur steam and the unreacted carbon oxideto the reactor to perform the cycling reaction; and condensing and collecting the carbonyl sulfide by a low-temperature collection tank, and then purifying in a purification system, thus obtaining high-purity carbonyl sulfide. By utilizing the metal sulfide as the catalyst, the reaction efficiency can be improved, and the unreacted raw material is recycled, so that the waste is avoided, and the difficulty for subsequently discharging harmful substances can be alleviated, and the cost is reduced; and for the characteristics of various impurities of a crude product, the corresponding purification means is adopted, so that the impurities in the carbonyl sulfide can be effectively removed.

Description

technical field [0001] The invention belongs to the technical field of industrial gas preparation, and relates to the preparation of carbonyl sulfide, in particular to a preparation method and a preparation device of carbonyl sulfide. Background technique [0002] Carbonyl sulfide (chemical formula: COS), also known as carbonyl sulfide and carbonyl sulfide, was first synthesized by Hungarian scientist Karoly Thanz in 1867. In 1970, Japan Ihara Chemical Industry Company first realized large-scale industrial production. It is a pesticide, medicine and other organic compounds. The important raw material gas synthesized can also be used as an important food fumigant and petrochemical standard gas raw material. In recent years, it has been found that high-purity carbon oxysulfide can be used as an etching gas for integrated circuit manufacturing to replace fluoride etching gas that is difficult to degrade and has a greenhouse effect. As governments of various countries pay more ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/77
CPCC01B32/77
Inventor 雷海平张建长吕其明
Owner 欧中汇智电子材料研究院(重庆)有限公司
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