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Method for monitoring and analyzing process of preparing 1, 3-cyclohexanedione through hydrogenation of resorcinol

A technology of cyclohexanedione and resorcinol, which is applied in the field of monitoring and analysis of the process of preparing 1,3-cyclohexanedione by hydrogenation of resorcinol, can solve problems such as insufficient analysis accuracy, and achieve good peak shape , Good repeatability and good peak shape

Pending Publication Date: 2022-03-18
中化河北有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The main purpose of the present invention is to provide a monitoring analysis method for the process of preparing 1,3-cyclohexanedione by hydrogenation of resorcinol, to solve the problem of the reaction product 1,3-cyclohexanedione or raw material in the prior art. The analysis of resorcinol, the accuracy of the analysis is insufficient, and only for the problem of analyzing the reaction product

Method used

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  • Method for monitoring and analyzing process of preparing 1, 3-cyclohexanedione through hydrogenation of resorcinol
  • Method for monitoring and analyzing process of preparing 1, 3-cyclohexanedione through hydrogenation of resorcinol
  • Method for monitoring and analyzing process of preparing 1, 3-cyclohexanedione through hydrogenation of resorcinol

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Experimental program
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Effect test

Embodiment 1

[0057] Resorcinol hydrogenation reaction process is as follows:

[0058] Put resorcinol, sodium hydroxide, water and catalyst into the autoclave, pass hydrogen into the autoclave, adjust to the appropriate pressure and temperature, and keep it until the end of the reaction. The feed liquid in the autoclave is taken out, the catalyst is removed by filtration, and the hydrogenation feed liquid is obtained. Use hydrochloric acid to adjust the pH value of the hydrogenation feed solution to about 2.5, and 1,3-cyclohexanedione crystals are precipitated, filtered, and dried to obtain 1,3-cyclohexanedione as a solid product.

[0059]The gas chromatography analysis process is as follows:

[0060] (1) Gas chromatography analysis conditions and parameters

[0061] The gas chromatograph was Shimadzu GC-2010Pro, the gas chromatographic column was Agilent DB-624 (0.25mm×30.0m, 1.4μm), and nitrogen was used as the carrier gas. The injection volume was 1.0 μL, the gasification chamber temp...

Embodiment 2

[0083] Compared with Example 1, the reverse-phase high performance liquid chromatography analysis condition part is adjusted as follows: the mobile phase is changed to V (acetonitrile: V (0.1% phosphoric acid aqueous solution)=20:80, and other conditions remain unchanged. Obtained The liquid chromatogram is as Figure 8 shown. It can be seen that under this condition, 1,3-cyclohexanedione and resorcinol are still well separated, and the peak shape still meets the requirements of quantitative analysis.

Embodiment 3

[0085] Compared with Example 1, the pH value of the mobile phase is adjusted to 4, and other conditions remain unchanged, and the liquid chromatogram obtained is as follows Figure 9 shown. Under this condition, the chromatographic peak shape of 1,3-cyclohexanedione is acceptable.

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Abstract

The invention provides a method for monitoring and analyzing the process of preparing 1, 3-cyclohexanedione through hydrogenation of resorcinol. The monitoring analysis step in the reaction process comprises the following steps: carrying out first reverse high performance liquid chromatography analysis on the first pretreated sample to obtain a first liquid chromatogram; obtaining the content of resorcinol and 1, 3-cyclohexanedione in a first sample to be analyzed according to the first liquid chromatogram; the monitoring analysis step after the reaction is finished comprises the following steps: firstly, carrying out gas chromatography analysis on the second pretreated sample to obtain a gas chromatogram, and carrying out qualitative analysis on component types in the second sample to be analyzed according to the gas chromatogram; then, sequentially carrying out third pretreatment and second reverse high performance liquid chromatography analysis on a second sample to be analyzed to obtain a second liquid chromatogram; and obtaining the content of resorcinol and 1, 3-cyclohexanedione in the second sample to be analyzed according to the second liquid chromatogram. According to the invention, the intermediate system and the reaction product can be comprehensively analyzed to obtain the reaction progress information.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for monitoring and analyzing the process of hydrogenating resorcinol to prepare 1,3-cyclohexanedione. Background technique [0002] 1,3-Cyclohexanedione is an important chemical intermediate that is widely used in organic synthesis. Catalytic hydrogenation of resorcinol is currently the most commonly used method for preparing 1,3-cyclohexanedione, and the common detection methods for reaction products mainly include gas chromatography and high performance liquid chromatography. [0003] Li Xinghua et al. ("Study on the Preparation of 1,3-Cyclohexanedione by Selective Hydrogenation of Resorcinol", Master Thesis of Zhejiang University, 2011; and "Analysis and Purification of Resorcinol Catalytic Hydrogenation Reaction Products", University Chemical Engineering Journal, 2011) the reaction product system was quantitatively analyzed by gas chromatography ( figure ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/89
CPCG01N30/02G01N30/06G01N30/14G01N30/89G01N2030/062G01N2030/146
Inventor 商建杨艳丽王晓晓张新琪宋楠楠
Owner 中化河北有限公司
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