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Analysis method of dimethyl oxalate

A technology of dimethyl oxalate and an analysis method, which is applied in the field of analysis of dimethyl oxalate, can solve the problems of dimethyl oxalate requiring heat treatment and cannot continuously automatically inject samples, and achieves the effect of improving analysis precision and efficiency

Pending Publication Date: 2022-07-29
SHAANXI WEIHE COAL CHEM GRP
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Problems solved by technology

[0004] The object of the present invention is to provide the analytical method of dimethyl oxalate, solve the problem that needs heat treatment and cannot continuous automatic sampling before detection of dimethyl oxalate in the prior art

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  • Analysis method of dimethyl oxalate
  • Analysis method of dimethyl oxalate
  • Analysis method of dimethyl oxalate

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Embodiment Construction

[0037] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

[0038] The invention provides an analytical method for dimethyl oxalate, which is specifically implemented according to the following steps:

[0039] Step 1, set gas chromatography parameters, and establish a dimethyl oxalate collection method:

[0040] Injection volume: 0.6ul, split ratio: 5:1, split flow 25ml / min, injection port temperature: 300℃;

[0041] Chromatographic column: DB624 60m×510um×3um, column flow: 5ml / min;

[0042]

[0043] Detector temperature: 300°C, air flow: 400ml / min, hydrogen flow: 40ml / min, makeup flow: 30ml / min;

[0044] Step 2, through the standard sample determination, establish the dimethyl oxalate treatment method:

[0045] Step 2.1, configuration of chromatographic standard:

[0046] Take 0.1 ml of methanol, methyl formate, ethanol, methylal, dimethyl carbonate, and 0.1 g of dimethyl oxalate in six 25 ml co...

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Abstract

The invention discloses a dimethyl oxalate analysis method which comprises the following steps: step 1, setting meteorological chromatographic parameters, and establishing a dimethyl oxalate acquisition method; step 2, establishing a treatment method of dimethyl oxalate through standard sample determination; step 3, sample analysis; the coal ethylene glycol intermediate product dimethyl oxalate has a melting point of 54 DEG C and is in a solid state at normal temperature. According to the method, acetonitrile is adopted as a solvent to dissolve solid dimethyl oxalate, so that the solid dimethyl oxalate can be directly injected on a gas chromatographic column head with an automatic sampler, and the purity and impurities of the dimethyl oxalate are detected through gas chromatographic separation.

Description

technical field [0001] The invention belongs to the technical field of dimethyl oxalate detection, in particular to an analysis method of dimethyl oxalate. Background technique [0002] Taking coal as raw material, CO and H are respectively obtained after gasification, transformation, purification and separation and purification. 2 , in which CO is synthesized by catalytic coupling of dimethyl oxalate, dimethyl oxalate and H 2 Hydrogenation reaction is carried out and polyester grade ethylene glycol is produced after refining. The technological process is short and the cost is low, and it is currently the main coal-to-ethylene glycol technology in China. [1] Dimethyl oxalate is an important intermediate product in production, and its quality directly affects the yield of ethylene glycol hydrogenation reaction. Therefore, it is extremely important to quickly and accurately detect the quality of dimethyl oxalate. [0003] Dimethyl oxalate has a melting point of 54°C and is ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/24
CPCG01N30/06G01N30/24
Inventor 陈卫陈小芬郭小龙高博伟毛梦雪
Owner SHAANXI WEIHE COAL CHEM GRP
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