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Method for detecting content of chloroacetic acid by using Raman spectrum

A technology of Raman spectrum detection and Raman spectroscopy, which is applied in the field of spectrum detection, can solve problems such as cumbersome detection process, poor reproducibility, and great impact on human health and the environment, and achieve significant economic benefits, accurate content prediction, and measurement short time effect

Pending Publication Date: 2022-04-22
杭州健澄科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this scheme overcomes the defects of chemical titration, such as complicated pre-treatment, consumption of a large amount of chemical reagents, great impact on human health and the environment, and poor reproducibility, it still cannot be solved when combined with ion chromatography for detection. The detection process is cumbersome, time-consuming and labor-intensive

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  • Method for detecting content of chloroacetic acid by using Raman spectrum
  • Method for detecting content of chloroacetic acid by using Raman spectrum
  • Method for detecting content of chloroacetic acid by using Raman spectrum

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Raman detection of chloroacetic acid, dichloroacetic acid and acetic acid standards using Raman spectroscopy

[0034] Use Raman spectrum to carry out Raman detection respectively to the standard substance of chloroacetic acid, dichloroacetic acid, acetic acid, obtain corresponding Raman spectrogram, as attached figure 1 shown, from figure 1 It can be seen that the Raman signal peaks of the three substances are obvious. The Raman spectrum test parameters are as follows:

[0035] Excitation light wavelength: 785nm, laser power: 500mw, detection time: 1s, cumulative times: 1 time.

[0036] (2) Use Raman spectroscopy to detect the sample in the production process of chloroacetic acid, and obtain the Raman spectrum of the sample.

[0037] Raman detection was performed on 21 samples using Raman spectroscopy. Each sample was detected 3 times, and the average spectrum of each sample was obtained. The concentration range of chloroacetic acid in the 21 samples is 70%-100...

Embodiment 2

[0050] According to the method substantially the same as Example 1, the Raman detection is carried out to the chloroacetic acid production process sample, the difference is: in step (2), the concentration of chloroacetic acid in the chloroacetic acid production process sample is 60%-90%, two The concentration of chloroacetic acid is 5%-30%, and the concentration of acetic acid is 5%-20%. The Raman spectrum detection parameters in step (2) are: excitation light wavelength: 633nm, laser power: 500mw, detection time: 5s, cumulative times: 2 times. In step (3), the preprocessing method is: smoothing, and the rest of the steps are the same as in Example 1. The result that obtains under this condition, the linear fitting degree of the real concentration of sample and predicted concentration is excellent, and deviation is also within the range described in above-mentioned embodiment 1, namely the relative deviation of chloroacetic acid is within ± 0.4%, dichloroacetic acid The relat...

Embodiment 3

[0052] Carry out Raman detection to the chloroacetic acid production process sample according to the method basically the same as embodiment 1, difference is: in the step (2) Raman spectrum detection parameter is: excitation light wavelength: 532nm, laser power: 500mw, detection time : 4s, accumulative times: 3 times. In step (3), the preprocessing method is: smoothing and K-S sample division method, all the other steps are the same as in Example 1, the result is obtained under this condition, the linear fitting degree of the true concentration of the sample and the predicted concentration is excellent , the deviation is also within the range described in the above-mentioned embodiment 1, that is, the relative deviation of chloroacetic acid is within ±0.5%, the relative deviation of dichloroacetic acid is within ±0.2%, and the relative deviation of acetic acid is within ±0.2%. .

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Abstract

The invention discloses a method for detecting the content of chloroacetic acid, dichloroacetic acid and acetic acid in a chloroacetic acid production process system by using Raman spectrum. Comprising the following steps: (1) carrying out Raman detection on a chloroacetic acid production process sample by using a Raman spectrometer, and collecting a Raman spectrum of the sample; (2) preprocessing the spectrum; (3) establishing a mathematical model between spectral data and corresponding contents of chloroacetic acid, dichloroacetic acid and acetic acid; and (4) predicting the content of chloroacetic acid, dichloroacetic acid and acetic acid in a to-be-detected sample by using the established mathematical model. The detection method is simple and rapid, and the economic benefit can be remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of spectral detection, and in particular relates to a method for detecting the content of chloroacetic acid by using Raman spectroscopy, in particular to a method for detecting chloroacetic acid and impurities dichloroacetic acid and acetic acid in the production process system of chloroacetic acid based on Raman spectroscopy. content method. Background technique [0002] Chloroacetic acid, also known as monochloroacetic acid, is an important organic chemical intermediate. There are active α-hydrogen, carboxyl, chlorine and other highly reactive functional groups in the molecule. It is an important fine chemical raw material, mainly used in pesticides, petrochemicals, pharmaceuticals, dyes and daily chemicals. With the rapid development and application of my country's petroleum industry and pesticide herbicides, the market demand for chloroacetic acid is constantly strong, and the industry is also developin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/65
Inventor 刘雅娇安志成孙海林李亚飞刘丽
Owner 杭州健澄科技有限公司