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Short-chain chlorinated paraffin online hydrogenation unit combined with gas chromatograph and application thereof

A technology of short-chain chlorinated paraffins and gas chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem that there is no method for analyzing the content of short-chain chlorinated paraffins, and it is difficult to accurately measure the content of short-chain chlorinated paraffins. Quantitative and other issues, to achieve the effect of shortening the analysis time, reducing the cost of the experiment, and easy operation

Active Publication Date: 2014-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are many analytical methods for short-chain chlorinated paraffins, such as high-resolution gas chromatography (HRGC) and high / low resolution mass spectrometry, comprehensive two-dimensional gas chromatography (GC×GC-electron capture negative chemical source (ECNI)- Rapid scanning quadrupole mass spectrometry (qTOF–MS), high performance liquid chromatography–chlorine-enhanced atmospheric pressure chemical ionization (CI–APCI) ion trap mass spectrometry, but due to the interference of a large amount of medium and long-chain chlorinated paraffins in chlorinated paraffin products, making The application of these methods to the analysis of short-chain chlorinated paraffins in chlorinated paraffin products has certain limitations, and it is difficult to accurately quantify
At present, there is no relevant standard for determining the content of short-chain chlorinated paraffins in chlorinated paraffin products in China, nor has an analysis method for the content of short-chain chlorinated paraffins in chlorinated paraffin products been established.

Method used

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  • Short-chain chlorinated paraffin online hydrogenation unit combined with gas chromatograph and application thereof
  • Short-chain chlorinated paraffin online hydrogenation unit combined with gas chromatograph and application thereof
  • Short-chain chlorinated paraffin online hydrogenation unit combined with gas chromatograph and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] like Figure 1~3 It is a structural schematic diagram of a short-chain chlorinated paraffin on-line catalytic dechlorination and hydrogenation device used in conjunction with a gas chromatograph, a structural schematic diagram of a catalyst loading method in a catalytic dechlorination and hydrogenation reaction tube, and the short-chain chlorinated paraffin is passed through the device of the present invention. The alkane gas chromatogram generated by the combination of gas chromatograph;

[0048] I ready status:

[0049] Quartz wool B, catalyst C 0.20g, calcium carbonate A, catalyst C 0.20g, calcium carbonate A and quartz wool B are packed in layers into the stainless steel reaction tube 301 of the catalytic dechlorination and hydrogenation reaction part 3, such as figure 2 shown. The interface part 5 is hermetically connected by a graphite gasket 503 . The interface part connected to the gas chromatograph is also sealed and checked for leaks. At this time, open t...

Embodiment 2

[0055] The experimental device and method conditions are the same as those in Example 1. A certain product of chlorinated paraffin, chlorowax-52, was used as the analysis object, and the n-hexane solution with a mass concentration of 5 g / L was prepared by the weighing method, and an internal standard substance was added. The inventive device performs catalytic dechlorination and hydrogenation and on-line analysis. The resulting chromatogram is Figure 4 shown. The determination was repeated 7 times, and the percentages of short-chain chlorinated paraffins in the total mass of chlorinated paraffins in the samples were 23.9%, 23.4%, 26.5%, 24.2%, 25.0%, 23.8%, 25.1%, 24.4% and 25.2%, respectively. The standard deviation is 3.8%. It shows that the device can be applied to the analysis and detection of the content of short-chain chlorinated paraffin in chlorinated paraffin products, and the method has high accuracy and good repeatability.

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Abstract

The invention relates to a short-chain chlorinated paraffin online hydrogenation unit combined with a gas chromatograph and a use method thereof. The short-chain chlorinated paraffin online hydrogenation unit comprises a sample feeding part, a carrier gas supplying part and a pressure controlling part, a catalysis dechlorinating and hydrogenating reaction part which is connected with the carrier gas supplying part and provided with a heating element, a temperature control part used for performing temperature control and regulation on the catalysis dechlorinating and hydrogenating reaction part, and an interface part connected with the gas chromatograph. An online catalysis dechlorinating and hydrogenating device is connected with a commercial gas chromatograph, and is used for performing data acquisition and analysis. The short-chain chlorinated paraffin online hydrogenation unit is used for performing online catalysis dechlorinating and hydrogenating on short-chain chlorinated paraffin, and has the advantages of accuracy in quantification, simple spectrum analysis, high analysis speed, low experimental cost, less health hazard, convenience in operation, and the like. The short-chain chlorinated paraffin online hydrogenation unit is suitable for routine laboratory analysis of the short-chain chlorinated paraffin in a chlorinated paraffin product.

Description

technical field [0001] The invention relates to an on-line catalytic dechlorination and hydrogenation device for short-chain chlorinated paraffin used in conjunction with a gas chromatograph for quantitative analysis of short-chain chlorinated paraffin in chlorinated paraffin products and a method for using the same. Specifically, a catalyst is used to efficiently convert short-chain chlorinated paraffins into corresponding alkanes under high temperature and high pressure conditions, and the pretreatment device and its use method are analyzed and quantified online by a gas chromatograph. Background technique [0002] Chlorinated paraffins (CPs) are a group of synthetic chlorinated derivatives of n-alkanes, mainly used as flame retardants for textiles, rubber and plastics, leather treatment agents, plasticizers for paints and other coatings, and metals Process oil additives. According to the different carbon chain length, it can be divided into short-chain chlorinated paraff...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14G01N30/02
Inventor 袁和平马潇阳高媛陈吉平张海军
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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