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A kind of assay method of unsaturated aldehyde content in liquid phase mixture

A determination method and mixture technology, which can be used in measurement devices, instruments, scientific instruments, etc., can solve the problems of loss of catalyst active components, decrease in catalyst activity, aggravation of by-products, etc., to reduce column pollution, improve reproducibility, The effect of reducing the influence of measurement results

Active Publication Date: 2019-07-05
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The gas-phase catalytic oxidation reaction of propylene to prepare acrolein and acrylic acid is a strong exothermic reaction, and a large amount of reaction heat is accumulated in the reactor instantaneously, forming local hot spots. If the reaction heat cannot be removed in time and effectively, the instantaneously accumulated heat will continue to accumulate, which will lead to catalyst The loss and detachment of active components lead to a decrease in catalyst activity and shortened life, and lead to the formation of by-products due to excessive oxidation reactions, and even lead to runaway reactions and sintering of catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 5890 chromatographic analysis conditions

[0047] Detector: hydrogen flame ionization detector (FID), chromatographic column: packed column 3mm * 3m, vaporization chamber temperature: 180 ℃, detector temperature: 190 ℃, carrier gas: (N 2 ) 50mL / min, hydrogen volume: 100mL / min, air volume: 30mL / min.

[0048] The reagents are commercially available products of analytical grade.

[0049] 1) Make a standard curve

[0050] Using methyl ethyl ketone as the internal standard, configure 6 acrolein standard solutions with concentrations ranging from 0.00010 to 0.00090 mol / L, accurately weigh to obtain the weight content of butanone and acrolein, and inject the standard solution into the gas chromatograph to obtain For the peak area of ​​butanone and acrolein, use the weight ratio of acrolein and internal standard as the ordinate, and the area ratio of acrolein and internal standard as the abscissa to make a standard curve, and obtain the relative correction factor f from the s...

Embodiment 2

[0055] The determination procedure is the same as in Example 1. The chromatographic column adopts non-isothermal temperature rise in stages, that is, it is kept at 110°C for 4 minutes, then the temperature is raised to 140°C at a heating rate of 25°C / min, and then the temperature is raised to 180°C at a heating rate of 10°C / min. The sampling bottle is condensed with 5°C water, C ACR =0.00086 mol / L.

Embodiment 3

[0057] The determination procedure is the same as that in Example 1. The chromatographic column adopts non-isothermal temperature rise in stages, that is, maintains 110°C for 1min, then raises the temperature to 140°C at a heating rate of 30°C / min, and then raises the temperature to 180°C at a heating rate of 10°C / min. The sampling bottle was condensed with a 0°C ice-water mixture. C ACR = 0.00075 mol / L.

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Abstract

The invention relates to a method for testing content of unsaturated aldehyde in a liquid phase mixture. The liquid phase mixture is mainly prepared from acrylaldehyde, propenoic acid and acetic acid. With butanone as an internal standard substance, the content of the unsaturated aldehyde in to-be-tested liquid is quantificationally analyzed by adopting an inner standardization method. The testing method disclosed by the invention has the advantages of low cost, simple and convenient operation, accurate test result and good repeatability.

Description

technical field [0001] The invention relates to a method for determining the content of unsaturated aldehyde in a liquid phase mixture, in particular to the determination of the content of acrolein in the liquid phase product of acrylic acid prepared by oxidation of acrolein. Background technique [0002] At present, acrylic acid is mainly produced in the industry by two-step oxidation of propylene, that is, a fixed-bed reactor is usually used, propylene is first oxidized to acrolein (one-stage reaction), and acrolein is oxidized to acrylic acid (two-stage reaction). [0003] In the research of catalysts for the preparation of acrolein (ACR) and acrylic acid (AA) from propylene, it is necessary to accurately detect the distribution and content of the reaction products, to screen the catalyst formula, investigate the life of the catalyst, and select the best catalyst. Process operating conditions, etc. provide reliable data. A liquid phase product is mainly acrolein, as well...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 刘俊保初伟吴毅曹帅英赵慧晖黄世英李淑萍魏玉丽翟月勤杜烨笪敏峰陈跟平
Owner PETROCHINA CO LTD