CN-122016711-A - Method for detecting hydrogen peroxide residue in N, N-diethyl hydroxylamine

Abstract

The invention belongs to the technical field of hydrogen peroxide detection, and discloses a method for detecting hydrogen peroxide residues in N, N-diethyl hydroxylamine. The detection method comprises the steps of preparing a series of samples of N, N-diethylhydroxylamine with different hydrogen peroxide concentrations, dividing the samples into a verification set and a training set, using a near infrared spectrometer to scan the samples of the verification set, establishing a data model, using the near infrared spectrometer to scan the samples of the training set, introducing the samples into the data model, verifying the accuracy, randomly selecting any sample, using the near infrared spectrometer to scan the sample for 2-10 times, verifying the repeatability, using the near infrared spectrometer to scan the sample to be detected, and introducing a near infrared spectrum file of the sample to be detected into the data model to obtain a predicted value. The invention adopts near infrared spectrum to detect, can detect the content of low-concentration hydrogen peroxide, has the advantages of simple operation, high precision, low detection limit, safety, environmental protection, high analysis speed, low cost and high efficiency.

Inventors

• FAN JIAN
• ZHANG XINNING
• XU SHUQUN
• WANG ZHENNI
• LIU CHENGLAN

Assignees

• 浙江圣安化工股份有限公司

Dates

Publication Date

20260512

Application Date

20260130

Claims (4)

1. 1. The method for detecting hydrogen peroxide residues in N, N-diethyl hydroxylamine is characterized by comprising the following steps: (1) The method comprises the steps of establishing a data model, namely preparing a series of samples of N, N-diethylhydroxylamine with different hydrogen peroxide concentrations, dividing the samples into a verification set and a training set, scanning the samples of the verification set by using a near infrared spectrometer, and establishing the data model according to a near infrared spectrum file of the samples of the verification set; (2) The method comprises the steps of adjusting a data model, namely scanning samples of a training set by using a near infrared spectrometer, introducing near infrared spectrum files of the samples of the training set into the data model, comparing predicted values of the data model with theoretical hydrogen peroxide concentration, and if the predicted values are within a standard range, performing subsequent detection; Randomly selecting any sample in the verification set or the training set, and scanning the sample for 2-10 times by using a near infrared spectrometer to verify repeatability; (3) And detecting a sample to be detected, namely taking N, N-diethyl hydroxylamine of residual hydrogen peroxide to be detected as the sample to be detected, scanning the sample to be detected by using a near infrared spectrometer, and introducing a near infrared spectrum file of the sample to be detected into a data model to obtain a predicted value, thereby finishing the detection of the hydrogen peroxide residue in the N, N-diethyl hydroxylamine.
2. 2. The method for detecting hydrogen peroxide residues in N, N-diethylhydroxylamine according to claim 1, wherein in the samples of the N, N-diethylhydroxylamine with different hydrogen peroxide concentrations in the step (1), the hydrogen peroxide concentration ranges from 0% to 15%.
3. 3. The method for detecting hydrogen peroxide residues in N, N-diethylhydroxylamine according to claim 1, wherein the quantitative ratio of the verification set to the training set in step (1) is 8:2.
4. 4. The method for detecting hydrogen peroxide residues in N, N-diethylhydroxylamine according to claim 1 or 3, wherein the standard range in the step (2) is R 2 not less than 0.9.

Description

Method for detecting hydrogen peroxide residue in N, N-diethyl hydroxylamine Technical Field The invention relates to the technical field of hydrogen peroxide detection, in particular to a method for detecting hydrogen peroxide residues in N, N-diethyl hydroxylamine. Background N, N-Diethylhydroxylamine (DEHA) is mainly used as a polymerization inhibitor for the production and storage of conjugated olefins such as styrene, divinylbenzene, butadiene, isoprene, acrylonitrile and other active bond-containing monomers. N, N-diethyl hydroxylamine is used as polymerization inhibitor, and has excellent polymerization inhibiting effect, no influence of temperature change on polymerization inhibiting efficiency, high polymerization inhibiting efficiency in liquid phase and excellent polymerization inhibiting performance in gas phase. The synthesis method of N, N-diethyl hydroxylamine is comparatively many, and from the industrial aspects of synthesis cost, raw material price, yield, product purity and the like, two most common methods for synthesizing N, N-diethyl hydroxylamine are a diethylamine oxidation method and a triethylamine oxidation cracking method. At present, most manufacturers at home and abroad mainly adopt a triethylamine oxidative cleavage method to produce N, N-diethyl hydroxylamine. The raw materials used in the two methods relate to hydrogen peroxide, and the residual amount of hydrogen peroxide in the N, N-diethyl hydroxylamine product is high and is easy to be dangerous, so that strict control is required. The existing method for detecting the H 2O2 content in hydrogen peroxide is mainly potassium permanganate or titration by an iodometric method, N-diethyl hydroxylamine in a system is used as a reducing agent, the existence of the N, N-diethyl hydroxylamine can interfere the titration result, and the titration method error is larger when H 2O2 is too low, so that the traditional method is not suitable for detecting the hydrogen peroxide content in the N, N-diethyl hydroxylamine. Titanium salt photometry (including potassium titanium oxalate, titanium sulfate, etc.) is also used for the detection of H 2O2, but it is required to be performed in an acidic environment, and N, N-diethylhydroxylamine is basic, and thus is not suitable. In view of the above, it is important to develop a method for detecting hydrogen peroxide residue in N, N-diethylhydroxylamine. Disclosure of Invention The invention aims to provide a method for detecting hydrogen peroxide residues in N, N-diethyl hydroxylamine, which solves the problem that the traditional detection method is not suitable for detecting the hydrogen peroxide content in N, N-diethyl hydroxylamine. In order to achieve the above object, the present invention provides the following technical solutions: the invention provides a method for detecting hydrogen peroxide residues in N, N-diethyl hydroxylamine, which comprises the following steps: (1) The method comprises the steps of establishing a data model, namely preparing a series of samples of N, N-diethylhydroxylamine with different hydrogen peroxide concentrations, dividing the samples into a verification set and a training set, scanning the samples of the verification set by using a near infrared spectrometer, and establishing the data model according to a near infrared spectrum file of the samples of the verification set; (2) The method comprises the steps of adjusting a data model, namely scanning samples of a training set by using a near infrared spectrometer, introducing near infrared spectrum files of the samples of the training set into the data model, comparing predicted values of the data model with theoretical hydrogen peroxide concentration, and if the predicted values are within a standard range, performing subsequent detection; Randomly selecting any sample in the verification set or the training set, and scanning the sample for 2-10 times by using a near infrared spectrometer to verify repeatability; (3) And detecting a sample to be detected, namely taking N, N-diethyl hydroxylamine of residual hydrogen peroxide to be detected as the sample to be detected, scanning the sample to be detected by using a near infrared spectrometer, and introducing a near infrared spectrum file of the sample to be detected into a data model to obtain a predicted value, thereby finishing the detection of the hydrogen peroxide residue in the N, N-diethyl hydroxylamine. Preferably, in the step (1), the concentration of hydrogen peroxide in the series of samples of N, N-diethylhydroxylamine with different concentrations of hydrogen peroxide is in a range of 0-15%. Preferably, the number ratio of the verification set to the training set in the step (1) is 8:2. Preferably, the standard range of the step (2) is R 2 to be more than or equal to 0.9. Compared with the prior art, the invention has the following beneficial effects: The invention provides a method for detecting hydrogen peroxide residues in N, N-diethyl hyd