Method for detecting coke deposition of catalyst by utilizing nuclear magnetic resonance

A technology of nuclear magnetic resonance and carbon deposition, which is applied in the direction of nuclear magnetic resonance analysis, etc., can solve the problems of slow detection speed, low detection accuracy, poor stability, etc.

Inactive Publication Date: 2013-07-10
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of low detection accuracy, slightly poor stability and slow detection speed in the detection of c

Method used

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  • Method for detecting coke deposition of catalyst by utilizing nuclear magnetic resonance
  • Method for detecting coke deposition of catalyst by utilizing nuclear magnetic resonance
  • Method for detecting coke deposition of catalyst by utilizing nuclear magnetic resonance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Using CP-MAS 13 The carbon spectra of 10 methanol-to-olefins SAPO-34 catalyst samples with known carbon content were detected by C NMR. The known sample is made by the catalyst evaluation device in the laboratory, and the amount of carbon deposit is analyzed by TG (thermogravimetric analyzer) in the laboratory. The amount of carbon deposition is controlled, so the distribution of the amount of carbon deposition of known samples obtained is not uniform.

[0029] Table 1 Known sample carbon deposition

[0030]

[0031] First, in order to eliminate the detection noise and effectively enhance the spectral information related to the component content, the raw spectral data was preprocessed with multivariate scatter correction.

[0032] Secondly, partial least squares regression and principal component regression were used to establish a correlation model between the carbon deposition amount and the peak area set of the sample, and the carbon deposition amount was predic...

Embodiment 2

[0036] Using CP-MAS 13 The carbon spectra of 10 methanol-to-propylene ZSM-5 catalyst samples with known carbon content were detected by C NMR. The known samples were prepared by the catalyst evaluation device in the laboratory, and the carbon deposition amount was analyzed by TG (thermogravimetric analyzer) in the laboratory. The known carbon deposition amount is shown in Table 3. Similarly, because the laboratory cannot perfectly control the carbon deposition amount according to the evaluation device, the distribution of the carbon deposition amount of the known samples obtained is not uniform.

[0037] Table 3 Known sample carbon deposition

[0038]

[0039] The same method as in Example 1 was used to establish a prediction model, and the results were predicted. The comparison between the predicted results and the actual results is shown in Figure 2, and the evaluation of the predicted results is shown in Table 4.

[0040] Table 4 Evaluation of prediction results

[00...

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Abstract

The invention discloses a method for detecting coke deposition of a catalyst by utilizing nuclear magnetic resonance. The method comprises the following steps of acquiring a carbon nuclear magnetic resonance spectrum of samples of certain quantity with known coke deposition, correlating and modeling a carbon spectrum peak area set and a coke deposition set of the known samples after being pretreated, and calculating the coke deposition of an unknown sample by predicting the carbon nuclear magnetic resonance spectrum of the model and the unknown sample. The method is fast, accurate and stable, can be used for offline detecting the coke deposition on a solid acid catalyst in the industry and is significant for optimizing a catalyst reaction-renewable system.

Description

technical field [0001] The invention relates to a method for detecting the carbon deposition amount of a catalyst, in particular to a method for detecting the carbon deposition amount of a catalyst by using carbon nuclear magnetic resonance spectroscopy. Background technique [0002] In the process of using solid acid catalysts to catalyze methanol to propylene, methanol to olefins, catalytic cracking, natural gas to olefins and olefins disproportionation, catalyst coking has been widely present. Catalyst coking refers to the process in which during the catalytic reaction of the catalyst, carbon deposits are formed on the surface or internal pores of the catalyst, which leads to the reduction or disappearance of the catalyst activity. Coke produced by industrial catalyst coking is mainly hydrocarbons, including aliphatic carbon, olefinic carbon and aromatic carbon. The industrial solution to catalyst carbon deposition is through coke regeneration. In the process of catalyst...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 王靖岱杨遥黄正梁王维群蒋云涛叶健廖祖维蒋斌波阳永荣
Owner ZHEJIANG UNIV
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