Method for detecting formaldehyde carbonylation reaction product by high performance liquid chromatography

A technology of high-performance liquid chromatography and carbonylation reaction, which is applied in the field of analytical chemistry, can solve the problems of gas chromatography, such as difficult gasification, low response value, and difficult analysis, and achieve the effects of small analysis error, high precision, and easy operation

Pending Publication Date: 2022-02-18
SHAANXI YANCHANG PETROLEUM GRP
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  • Description
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Problems solved by technology

[0002] The synthesis of ethylene glycol by formaldehyde carbonylation has the advantages of green process, atom economy, few technical links and auxiliary units, and low separation cost, so it is considered to be a promising synthetic route for ethylene glycol. High (197.3°C), it is not easy to gasify by gas chromatography, and it is difficult to analyze; and there are a series of by-products glycolic acid, ethylene glycol, glyoxylic acid, acetic acid, acetaldehyde and the reaction raw material formaldehyde in this reaction, all of which are present in gas chromatography Therefore, a complete set of high performance liquid chromatography analysis methods for formaldehyde carbonylation reaction products glycolic acid, ethylene glycol, glyoxylic acid, acetic acid, acetaldehyde and formaldehyde were established to realize these The effective separation and accurate quantification of compounds is of great significance for the formaldehyde-based ethylene glycol route

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  • Method for detecting formaldehyde carbonylation reaction product by high performance liquid chromatography
  • Method for detecting formaldehyde carbonylation reaction product by high performance liquid chromatography
  • Method for detecting formaldehyde carbonylation reaction product by high performance liquid chromatography

Examples

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Embodiment 1

[0034] A method for detecting formaldehyde carbonylation reaction products by high performance liquid chromatography, comprising the following steps:

[0035] (1) Preparation of liquid chromatography mobile phase:

[0036] Take methanol or acetonitrile, filter through an organic membrane, and use ultrasonic treatment for 10-30 minutes as the organic phase; take ultrapure water, filter with an aqueous membrane filter, and use ultrasonic treatment for 10-30 minutes as the aqueous phase;

[0037] (2) Preparation of mixed standard stock solution:

[0038] Weigh glycolic acid, ethylene glycol, glyoxylic acid aqueous solution, acetic acid, acetaldehyde and formaldehyde aqueous solution in volumetric flasks respectively, use organic solvent to constant volume, shake up 1-2min, obtain mixed standard stock solution; In the solution, the concentration of each component is as follows: glycolic acid 10-200μg / mL, ethylene glycol 10-200μg / mL, glyoxylic acid 5-200μg / mL, acetic acid 10-200μg...

Embodiment 2

[0049] On the basis of Example 1, the chromatographic conditions are established as follows:

[0050] The chromatographic column is one of C18 chromatographic column, porous silica gel chromatographic column, and C8 chromatographic column; the diameter of the chromatographic column is 1-5mm, the length is 10-50mm, and the particle size is 1-5μm; the elution method is isocratic elution; in the mobile phase The proportion of the organic phase is 30%-70%, and the rest is the aqueous phase; the temperature of the column oven is 10-50°C; the flow rate is 0.5-5mL / min; the injection volume is 5-20μL; the detection is an ultraviolet detector with a wavelength of 200-400nm.

[0051] The concentration of the glyoxylic acid aqueous solution is 50wt%, and the concentration of the formaldehyde aqueous solution is 40wt%.

[0052] Preferably, the organic membrane is a 0.22 μm nylon filter membrane or a 0.22 μm PTFE filter membrane, and the water-based filter membrane is a 0.22 μm MCE filter...

Embodiment 3

[0054] A method for detecting formaldehyde carbonylation reaction products by high performance liquid chromatography, comprising the following steps:

[0055] (1) Preparation of liquid chromatography mobile phase:

[0056] Take 500mL of methanol, filter with a 0.22μm nylon filter membrane, sonicate for 10min, and use it as the organic phase; take 500mL of ultrapure water, filter with a 0.22μmMCE filter membrane, and use ultrasonic treatment for 10min as the aqueous phase;

[0057] (2) Preparation of mixed standard stock solution:

[0058] Weigh 1mg glycolic acid, 1mg ethylene glycol, 1mg 50wt% glyoxylic acid aqueous solution, 1mg acetic acid, 1mg acetaldehyde and 10mg 40wt% formaldehyde aqueous solution in a 100mL volumetric flask, dilute to volume with ethanol, shake well for 1-2min , to obtain a mixed standard stock solution; in the mixed standard stock solution, the concentration of each component is as follows: glycolic acid 10 μg / mL, ethylene glycol 10 μg / mL, glyoxylic a...

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Abstract

The invention discloses a method for detecting a formaldehyde carbonylation reaction product by high performance liquid chromatography. The method comprises the following steps: (1) preparing a liquid chromatography mobile phase; (2) preparing a mixed standard stock solution, namely respectively weighing glycollic acid, ethylene glycol, a glyoxylic acid aqueous solution, acetic acid, acetaldehyde and a formaldehyde aqueous solution, putting into a volumetric flask, fixing the volume by using an organic solvent, and uniformly shaking to obtain the mixed standard stock solution; (3) preparation of standard solutions: respectively taking 5 parts of the mixed standard stock solution in the step (2), putting the mixed standard stock solution into the volumetric flask, fixing the volume by using an organic solvent, and uniformly shaking to obtain 5 series of standard solutions with different concentrations; (4) establishment of chromatographic analysis conditions; (5) making a standard curve: performing liquid chromatographic analysis, and fitting by taking the concentration as an abscissa and the peak area as an ordinate to obtain the standard curve; and (6) analyzing a reaction product. The method provided by the invention is simple and convenient to operate, good in repeatability, small in analysis error, high in precision and good in sensitivity.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for detecting formaldehyde carbonylation reaction products by high-performance liquid chromatography. Background technique [0002] The synthesis of ethylene glycol by formaldehyde carbonylation has the advantages of green process, atom economy, few technical links and auxiliary units, and low separation cost, so it is considered to be a promising synthetic route for ethylene glycol. High (197.3°C), it is not easy to gasify by gas chromatography, and it is difficult to analyze; and there are a series of by-products glycolic acid, ethylene glycol, glyoxylic acid, acetic acid, acetaldehyde and the reaction raw material formaldehyde in this reaction, all of which are present in gas chromatography Therefore, a complete set of high performance liquid chromatography analysis methods for formaldehyde carbonylation reaction products glycolic acid, ethyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/04G01N30/06G01N2030/042
Inventor 张磊郭淑静葛元征袁亚飞陈佑涛
Owner SHAANXI YANCHANG PETROLEUM GRP
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