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On-line chromatographic analytical system and use for gas-solid-phase oxidation reactant

An oxidation reaction and chromatographic analysis technology, which is applied to the online chromatographic analysis system of gas-solid phase oxidation reaction products and its application field, can solve the problems of long analysis time, inability to analyze oxygen, errors, etc., and achieve the effect of fast and accurate analysis

Active Publication Date: 2006-08-16
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another method is to add a Ni reduction column in front of the chromatographic column to reduce carbon monoxide and carbon dioxide into methane, then detect it with a hydrogen flame detector, and use the external standard method for quantification. This method can only analyze carbon monoxide and carbon dioxide, but not Analyzing the incompletely reacted oxygen, and there are large errors in the quantification by external standard method for manual injection
[0003] In addition, after analyzing the organic oxidation products and inorganic oxidation products (carbon monoxide and carbon dioxide) separately, only the content of each substance in the respective sample system can be obtained
Since the two samples cannot be effectively linked, it is also difficult to calculate the carbon balance data of the oxidation reaction, and multiple injections are required to complete the entire analysis, the analysis time is long, the operation is complicated, and large experimental errors are prone to occur

Method used

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  • On-line chromatographic analytical system and use for gas-solid-phase oxidation reactant
  • On-line chromatographic analytical system and use for gas-solid-phase oxidation reactant
  • On-line chromatographic analytical system and use for gas-solid-phase oxidation reactant

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Embodiment 1

[0023] see Figure 1 ~ Figure 3 . The two-step oxidation of isobutene or tert-butanol to methacrylic acid is a typical complex gas-solid phase oxidation reaction. At this time, isobutene or tert-butanol and air pass through a fixed-bed shell-and-tube reactor equipped with a solid catalyst to undergo an oxidation reaction. The product of this reaction is more complicated, except the unreacted isobutene (i-C 4 ) and deep oxidation products carbon monoxide (CO), carbon dioxide (CO 2 ), there are organic oxidation products such as methacrolein (MAL), methacrylic acid (MAA), acetaldehyde, propionaldehyde, acetone, acrolein, acetic acid, propionic acid and acrylic acid. use figure 1 The shown online analysis system of the present invention analyzes the oxidation product of this reaction, and the composition of the system includes: sample inlet and outlet, two carrier gas flow lines, four chromatographic columns, thermal conductivity detector and hydrogen flame ion chemical dete...

Embodiment 2

[0028] The two-step oxidation of propylene to acrylic acid is also a typical complex gas-solid phase oxidation reaction. Propylene passes through a fixed-bed shell-and-tube reactor equipped with a solid catalyst for oxidation reaction. Oxidation products of this reaction include carbon monoxide, carbon dioxide, propylene, acetaldehyde, propionaldehyde, acetone, acrolein, acetic acid, propionic acid, and acrylic acid, among others. Adopt the online analysis system of the present invention identical with embodiment 1 to analyze the oxidation product of this reaction, chromatographic column 1, chromatographic column 2, chromatographic column 3 and chromatographic column 4 select PEG-20M packed column, Porapak Q packed column respectively , 5A molecular sieve packed column and FFAP capillary column. The qualitative analysis chromatograms of each substance are shown in Figure 5 and 6 , ethanol was selected as the associated substance for quantitative analysis. At the same time...

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Abstract

An on-line chromatographic analysis system of gas-solid phase oxidizing reaction product comprises sample inlet and outlet, two carrier airflow pipelines four pieces of chromatographic columns, heat conduction detector and hydrogen flame ionization detector. It is featured as connecting said system to two sets of different reaction units and setting two six-way valves and one ten-way valve in said system for switching over these valves to realize separation and detection of multicomposition.

Description

technical field [0001] The invention relates to a device system for controlling and detecting chemical reaction process in chemical production and its application, in particular to an on-line chromatographic analysis system of gas-solid phase oxidation reaction product and its application. Background technique [0002] As we all know, gas-solid phase oxidation reaction is involved in many chemical processes (for example, producing acid from olefin oxidation, etc.), and timely grasping the process of this reaction is one of the keys to controlling the entire process. Therefore, it is required to Gas-solid phase reaction products have a timely understanding. Gas-solid phase oxidation reaction products mainly include target oxidation products and organic by-products, carbon monoxide, carbon dioxide, unreacted oxygen, inert gas or diluent gas nitrogen, etc. At present, the main method of analyzing these oxidation products is to collect the organic products by condensation or ab...

Claims

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Application Information

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IPC IPC(8): G01N30/20G01N30/60G01N30/88
Inventor 成启刚庄岩张春雷李军温新袁海英
Owner SHANGHAI HUAYI NEW MATERIAL
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