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Analysis method for reaction products of preparing ethylene glycol by ethylene oxide catalytic hydration

A technology of ethylene oxide catalyzing water and reaction products, which is applied in the direction of analyzing materials, material separation, and measuring devices, can solve problems such as heavy peaks in chromatographic peaks, poor repeatability of analysis results, etc., and achieve high analysis accuracy and precision, Eliminates the effect of large volume expansion and good technical effects

Active Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is that in the prior art, when there is a large amount of water in the analyte containing ethylene glycol, the chromatographic peaks are heavy, bifurcated, and the repeatability of the analysis results is poor. A new ethylene oxide is provided Gas Chromatography Analysis Method of Catalytic Hydration to Ethylene Glycol Reaction Products

Method used

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  • Analysis method for reaction products of preparing ethylene glycol by ethylene oxide catalytic hydration
  • Analysis method for reaction products of preparing ethylene glycol by ethylene oxide catalytic hydration
  • Analysis method for reaction products of preparing ethylene glycol by ethylene oxide catalytic hydration

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Effect test

Embodiment 1

[0018] Preparation of filled Tenax TA glass liners:

[0019] The liner adopts the split / splitless glass liner from Agilent, which has a partition in the middle and a tapered bottom. Fill the bottom of the liner with silanized glass wool 2-3 mm, and after flattening, fill Tenax TA (60-80 mesh) 21-22 mm on the top, then fill the glass wool to the interrupted part of the liner, and flatten it.

[0020] Ageing:

[0021] Put the glass liner loaded with Tenax TA into the gas chromatograph inlet, use high-purity nitrogen as the carrier gas, set the chromatographic conditions as follows: detector temperature 250°C, column front pressure 20psi, carrier gas linear velocity 37cm s -1 , split ratio 30:1, gas 32mL / min, assisted gas 350mL / min, auxiliary gas 25mL / min, oven temperature 160°C, gasification chamber temperature at room temperature, after 20 minutes of stabilization, set the gasification chamber temperature to 250 ℃, using temperature programming, the initial temperature is 160...

Embodiment 2

[0039] After the completion of Example 1, the conditions were unchanged (the 1mL syringe was the corresponding syringe in Example 1), about 3mL samples were taken from the ethylene glycol catalytic hydration process device of ethylene oxide with a 5mL sampling bottle, and 1mL Accurately extract 1mL sample with 1mL internal standard 6% ethylene glycol butyl ether aqueous solution and mix evenly, use 1 μ L microsampler (needle length is identical with embodiment 1), get 0.2 μ L and inject gas chromatographic inlet and analyze, analyze The results are shown in Table 4 (the FID detector does not have a peak for water).

[0040] Table 4

[0041] keep time

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Abstract

The invention relates to an analysis method for reaction products of preparing ethylene glycol by ethylene oxide catalytic hydration, which is mainly used for solving the problems of overlapped peak and furcation of chromatographic peak in the presence of a large amount of water as well as poor analysis result repeatability in the existing glycol, diethylene glycol and triethylene glycol analysistechnology. The technical scheme of the analysis method of the invention is as follows: a gas chromatograph is used to perform the analysis, wherein the reaction product passes through Tenax TA polymeric adsorbent before entering into the chromatographic column, and then the follow-up analysis is carried out; and the internal standard substance is a butyl cellosolve aqueous solution, thus the problems in the prior art can be preferably solved, and the analysis method can be used for tracking and analyzing the technological products for preparation of ethylene glycol by ethylene oxide catalytic hydration.

Description

technical field [0001] The invention relates to an analysis method for the reaction product of ethylene glycol prepared by catalytic hydration of ethylene oxide. Background technique [0002] Ethylene glycol, also known as glycol, is an important petrochemical basic organic raw material, mainly used in the production of polyester fibers, antifreeze agents, unsaturated polyester resins, lubricants, plasticizers, nonionic surfactants and explosives Wait. At present, the industrial production methods of ethylene glycol at home and abroad are mainly ethylene oxide direct hydration method, ethylene oxide catalytic hydration method, ethylene carbonate method, and various new production methods such as synthesis of ethylene glycol from synthesis gas. Ethylene oxide hydration to ethylene glycol process, although many companies are doing research, but there is no literature report on the product analysis method of ethylene oxide hydration to ethylene glycol process. [0003] The ma...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/28G01N30/56
Inventor 肖含何文军王嘉华何立费泰康
Owner CHINA PETROLEUM & CHEM CORP
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