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High-flux packed chromatographic column for detecting sulfide in hydrogenated benzene and application thereof

A technology for filling chromatographic columns and sulfides, which is applied in the field of gas chromatography detection, can solve the problems of simultaneous determination of hydrogen sulfide thiophene, cannot meet user needs, and low measurement accuracy, and achieves improved selective separation performance, simple structure, and detection accuracy high effect

Inactive Publication Date: 2020-02-11
TANGSHAN ZHONGRUN COAL CHEM CO LTD
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

However, the above three methods cannot simultaneously determine the content of hydrogen sulfide, carbonyl sulfide, propanethiol and thiophene, and the measurement accuracy is low. Only the spectrophotometric method can measure 0.1mg / kg thiophene, and the minimum detection line of the other two methods is 1mg / kg total sulfur cannot meet the needs of benzene hydrogenation production enterprises and downstream enterprise users

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  • High-flux packed chromatographic column for detecting sulfide in hydrogenated benzene and application thereof
  • High-flux packed chromatographic column for detecting sulfide in hydrogenated benzene and application thereof
  • High-flux packed chromatographic column for detecting sulfide in hydrogenated benzene and application thereof

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Effect test

Embodiment approach 1

[0040] The large-throughput packed chromatographic column for detecting sulfide in hydrogenated benzene provided by this method, such as figure 1As shown, it includes: a hollow column tube 2, the two ends of the hollow column tube 2 are respectively filled with quartz wool 4 to block the hollow column tube 2, and the hollow column tube 2 is filled with a porous silica gel carrier 6, so The surface of the porous silica gel carrier 6 is coated with a fixative solution layer 8, and the fixative solution layer 8 is tetracyanoethyl pentaerythritol fixative solution.

[0041] This method can solve the current technical problems that the detection accuracy of sulfides in hydrogenated benzene is low and the detection effect of sulfide types is relatively limited.

[0042] This method can separate hydrogen sulfide, carbonyl sulfide, propanethiol, thiophene and hydrogenated benzene through the strong polarity of tetracyanoethyl pentaerythritol fixative, and obtain more types of detectio...

Embodiment approach 2

[0052] The large-throughput packed chromatographic column for detecting sulfide in hydrogenated benzene provided by this method includes: a high borosilicate hollow column tube 2, the tube length of which is 3.1m and the inner diameter is 3mm The two ends of the high borosilicate hollow column tube 2 are respectively filled with quartz wool 4 to block the hollow column tube 2, and the hollow column tube 2 is filled with dimethylchlorosilane (DMCS) after inert treatment. The porous silica gel carrier 6, the porous silica gel purity of the porous silica gel carrier 6 is 99%, the particle size of the porous silica gel carrier 6 is 80-100 mesh, and the specific surface area is 4-6m 2 / g; the surface of the porous silica gel support 6 is coated with a stationary liquid layer 8, and the stationary liquid layer 8 is a tetracyanoethyl pentaerythritol stationary liquid, and the tetracyanoethyl pentaerythritol stationary liquid and the porous silica gel support The mass ratio of 6 is 1....

Embodiment approach 3

[0055] The quantitative detection method for sulfide in hydrogenated benzene provided by this embodiment uses the above-mentioned large-throughput packed chromatographic column for detecting sulfide in hydrogenated benzene, and the sulfide is hydrogen sulfide, carbonyl sulfide, propanethiol and thiophene one or more, including the following steps:

[0056] (1) Get the hydrogenated benzene sample to be detected, use a gas chromatograph to separate and detect, and record the chromatogram for at least 10 minutes, wherein the operating conditions of the gas chromatograph are as follows:

[0057] The chromatographic column adopts the large-throughput packed chromatographic column for detecting sulfide in hydrogenated benzene in the second embodiment; the injection volume is 25 μL, and the sample is splitless; the temperature of the injection port is 150 ° C; The column oven temperature: 80°C-81.5°C; the temperature rise program is an initial temperature of 80°C, rising to 81.5°C at...

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Abstract

The invention relates to a high-flux packed chromatographic column for detecting sulfide in hydrogenated benzene and application thereof, and belongs to the technical field of gas chromatographic detection. The high-flux packed chromatographic column for detecting sulfide in hydrogenated benzene comprises a hollow column tube, the two ends of the hollow column tube are filled with quartz wool respectively, the hollow column tube is filled with a porous silica gel supporter, the surface of the porous silica gel supporter is coated with a stationary liquid layer, and the stationary liquid layeris tetracyanoethyl pentaerythritol stationary liquid. The invention also discloses a method for quantitatively detecting sulfide in hydrogenated benzene by using the chromatographic column for detecting sulfide in hydrogenated benzene. The chromatographic column disclosed by the invention can be used for quantitatively detecting the contents of hydrogen sulfide, carbonyl sulfide, propanethiol andthiophene in hydrogenated benzene, and is high in sensitivity, good in repeatability, good in recovery rate, high in detection precision, simple in structure and quick and convenient, and more sulfidetypes can be detected.

Description

technical field [0001] The invention belongs to the technical field of gas chromatography detection, in particular to a large-throughput packed chromatographic column for detecting sulfide in hydrogenated benzene and an application thereof. Background technique [0002] Hydrogenated benzene is an important basic organic chemical raw material, which is widely used in fine chemical intermediates and organic raw materials. The sulfur content in hydrogenated benzene is relatively low, and sulfur mainly exists in the form of sulfides such as hydrogen sulfide, carbonyl sulfide, propanethiol and thiophene. The level of sulfur content directly affects the catalyst life of downstream deep processing enterprises. High sulfur content will lead to catalyst poisoning. Therefore, sulfur content is strictly limited in downstream enterprises of hydrogenated benzene, especially in industries that require adipic acid and caprolactam. The requirements for thiophene in the medium are relativel...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/60G01N30/74
CPCG01N30/06G01N30/60G01N30/74
Inventor 李小亮王冬冬谷志强凡立辉张宏亮卜雪锋刘慧蒋嗣颖周正
Owner TANGSHAN ZHONGRUN COAL CHEM CO LTD
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