Method for analyzing content of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane based on Raman spectrum

Abstract

The invention discloses a method for analyzing the content of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane based on a Raman spectrum, and belongs to the technical field of detection, and the method comprises the following steps: (1) obtaining Raman spectrum diagrams of n samples with known content data; (2) comparing the obtained gas chromatographic data of the n samples with the known content data with the Raman spectrograms of the n samples with the known content data, and establishing a model relationship between the gas chromatographic data and the Raman spectrograms by utilizing chemometrics software; (3) comparing the obtained gas chromatographic data of the n to-be-detected samples with the content data of the n to-be-detected samples obtained according to the model relationship, and correcting and optimizing the Raman spectrum model; and (4) a Raman spectrum model is utilized to perform online continuous monitoring, so that a result is obtained quickly, the reproducibility is good, the accuracy rate is high, and the situation that 101 is decomposed in the synthesis and heat preservation process due to too long analysis time can be reduced.

Description

Technical Field

[0001] This invention belongs to the field of detection technology and relates to a method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy. Background Technology 2,5-Dimethyl-2,5-di(tert-butylperoxy)hexane (abbreviated as 101) is an important organic peroxide in industry. It has a molecular weight of 290.5, a specific gravity (D at 20℃) of 0.865, a refractive index of 1.4185, a flash point of 36℃ (closed cup) and 58℃ (open cup), an alarm temperature of 75℃, an auto-accelerating decomposition temperature of 80℃, and a theoretical active oxygen content of 11.02%. It is a flammable, explosive, odorless, pale yellow, transparent, oily liquid. 2,5-Dimethyl-2,5-di(tert-butylperoxy)hexane is commonly used as a free radical initiator in polymerization processes and to improve the viscosity of polyolefins. It is also used in silicone rubber vulcanization products. Due to its high tensile strength and hardness, and low elongation and compression set, it is used as an effective high-temperature vulcanizing agent for vinyl rubber, a curing agent for unsaturated polyesters, and a vulcanizing agent for materials such as fluororubber, polyurethane rubber, and ethylene propylene rubber.

[0002] Currently, the detection method for 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane is gas chromatography, which takes approximately 20-30 minutes and results in a relatively long data output time. Since prolonged exposure to heat during synthesis can lead to the decomposition of 101, affecting product yield, the development of a rapid detection method is crucial.

[0003] Raman spectroscopy is based on the Raman scattering effect. When a light beam illuminates molecules, most of the scattered light has a constant frequency, which is called Rayleigh scattering; a very small portion of the scattered light has a different frequency than the incident light, which is called Raman scattering. This frequency change is related to the vibration and rotation of molecules.

[0004] The horizontal axis of a Raman spectrum represents the Raman shift, measured in cm. -1 The wavenumber, also known as the Raman shift, is the frequency difference between the scattered Raman light and the incident light. The Raman shift is related to the vibrational modes and structure of molecules and can be used to analyze the types of chemical bonds and molecular structure of substances.

[0005] The vertical axis of a Raman spectrum represents Raman scattering intensity, a dimensionless unit that refers to the intensity of Raman light. Raman scattering intensity is related to the vibrational intensity of molecules and the molar concentration of molecules within the system, and can be used to quantitatively analyze the content of various molecules in a mixture.

[0006] Therefore, developing a Raman spectroscopy-based method for the analysis of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content that is simple to operate, highly efficient, and provides accurate data is a technical problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0007] In view of this, the present invention provides a method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy.

[0008] To achieve the above objectives, the present invention adopts the following technical solution: A method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy includes the following steps: (1) Raman spectra of n 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with known content data were determined by Raman spectrometer. (2) The 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with n known content data from step (1) were determined by gas chromatography and chemical analysis. The gas chromatography data of the n samples with known content data were compared with the Raman spectra of the n samples with known content data obtained in step (1). A model relationship between the two was established using chemometrics software. The model relationship between the two is as follows:

[0009] Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. This represents the spectral fitting region, and N represents the number of Lorentz peaks. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. (3) Use a Raman spectrometer to determine the content data of n samples to be tested. According to the model relationship in step (2), obtain the content data of n samples to be tested. Then use gas chromatography and chemical analysis to determine the content data of n samples to be tested. Compare the gas chromatography data of the n samples to be tested with the content data of the n samples to be tested obtained according to the model relationship in step (2). Perform adaptive baseline subtraction on the Raman spectrum of the sample to be tested to correct it. Perform Lorentz peak fitting and peak separation on the corrected Raman spectrum to extract the characteristic peaks of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane and the single-sided oxide 5-tert-butylperoxide-2,5-dimethylhexane-2-ylhydrogen peroxide. Calculate the peak area of ​​the corresponding characteristic peak. Correlate the obtained peak area with the peak area obtained by gas chromatography to find its functional relationship. Correct and optimize the Raman spectral model. For points with large deviations, increase the sampling amount and subtract points with large deviations. Refit. The corrected Raman spectral model is:

[0010] Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. Indicates the spectral fitting region. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. (4) During the stirring reaction of materials in the reactor, some materials are collected by diaphragm pump and automatically separated in oil-water separator. Due to the different densities of oil and water, the crude oil phase material 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane flows back into the reactor through the upper oil phase overflow pipe, while the lower water phase material synthesis mother liquor returns to the reactor through the water phase balance pipe. The Raman spectrometer detection probe extends from the upper end of the oil-water separator into the crude oil phase material 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane and uses the Raman spectroscopy model established in step (3) for online continuous monitoring. In steps (1)-(3), n≥20.

[0011] Furthermore, in step (1), the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane sample with known content data has a 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content of 60~85% and a single-sided oxide content of 0~20%.

[0012] Furthermore, in steps (2) and (3), the gas chromatographic data of 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane were determined in accordance with T / CPCIF 0021-2018 "Industrial 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane".

[0013] Furthermore, in steps (1) and (3)-(4), the detection conditions of the Raman spectrometer are: integration time of 1000-20000ms, number of sampling points of 3-8, and number of dark spectrum acquisitions of 1-3.

[0014] Furthermore, in steps (1) and (3)-(4), the number of scans for each sample is determined by Raman spectrometer not less than 3 times.

[0015] Furthermore, in step (4), the Raman spectrometer is set to work continuously. After one detection is completed, the second detection will start automatically. Each detection takes 4-220 seconds. The reaction system is continuously detected during the reaction process and the detection results are obtained in real time.

[0016] The present invention has the following beneficial effects: In this invention, a model relationship was established between the Raman spectrum of sample 101 and the content of 101 and impurities. This allows for continuous online monitoring using Raman spectroscopy during the reaction in the workshop, and the content can be obtained by using the model relationship. The results are rapid, reproducible, and accurate, and can reduce the decomposition of 101 during the synthesis and heat preservation process due to excessive analysis time.

[0017] Step (4) Raman spectroscopy yields results faster, with shorter waiting times, and allows for quicker determination of the reaction endpoint.

[0018] By monitoring the composition and content of materials during the reaction process online in real time, incomplete or excessive reactions can be prevented from affecting product quality and production efficiency can be improved.

[0019] In actual production at the workshop, Raman spectroscopy can be used for online monitoring of the reaction system. A small-flow external circulation system is connected to the workshop reactor, with an integrated oil-water separator on the circulation pipeline. By adjusting the external circulation flow rate, the presence of clearly defined oil and water phases in the separator is controlled. The Raman spectroscopy probe is inserted into the oil phase in the separator for continuous online monitoring. Each detection integration time is 1000–20000 ms, with 3–8 sampling points and 1–3 dark spectrum acquisitions, completing one detection cycle in approximately 4–220 seconds. Traditional gas chromatography methods take 20–30 minutes; in comparison, Raman spectroscopy provides faster results and more rapid determination of the reaction endpoint, reducing the time required for the decomposition of oxide 101 during the waiting period. Furthermore, online monitoring throughout the entire reaction process allows for a more intuitive and clearer view of the changing trends in the content of each component. Multiple consecutive measurements yield multiple sets of data, reducing errors and making the results more accurate. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0021] Figure 1 This is a flowchart illustrating the online continuous monitoring of the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content in the reactor using the Raman spectrometer of this invention. Figure 2 Raman spectra of 20 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples to be tested; Figure 3 The discreteness of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content in step (3) of establishing the Raman spectral model for this invention; Figure 4 Step (3) of establishing the Raman spectral model for this invention: the discreteness of the single-sided oxide content. Detailed Implementation

[0022] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] Example 1 Establishing a Raman spectral model: (1) Raman spectra of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with known content data were determined by Raman spectrometry. The Raman spectra of the 25 samples with known content data were obtained. The content of 101 in sample with known content data was 60~85%, and the content of single oxide (5-tert-butylperoxide-2,5-dimethylhexane-2-ylhydrogen peroxide, CAS No.: 23661-84-9) was 0~20%.

[0024] Table 1. Raman content of 25 samples with known content data

[0025] The detection conditions using the Raman spectrometer were: integration time of 8000 ms, number of sampling points of 4, and number of dark spectrum acquisitions of 1. Each sample was scanned 5 times using the Raman spectrometer.

[0026] (2) The contents of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with known content data in step (1) were determined by gas chromatography and chemical analysis.

[0027] Table 2. GC content of 25 samples with known content data

[0028] The gas chromatographic data of the 25 samples with known content were compared with the Raman spectra of the 25 samples with known content obtained in step (1). A model relationship between the two was established using chemometrics software. The model relationship is as follows:

[0029] Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. This represents the spectral fitting region, and N represents the number of Lorentz peaks. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. 101 gas chromatographic data were obtained according to T / CPCIF 0021-2018 "Industrial grade 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane".

[0030] (3) Raman spectroscopy was used to measure 20 samples, such as... Figure 2 As shown, the content data of 20 samples to be tested were obtained according to the model relationship in step (2), and then the content of 20 samples to be tested was determined by gas chromatography and chemical analysis.

[0031] Table 3. Raman and GC content of 20 samples to be tested.

[0032] Table 4. Raman spectroscopy and GC content of unilateral oxides in 20 samples.

[0033] The gas chromatographic data of the 20 test samples were compared with the content data of the 20 test samples obtained according to the model relationship in step (2). The Raman spectra of the test samples were corrected by adaptive baseline subtraction. The corrected Raman spectra were then fitted with Lorentz peaks and separated to extract the characteristic peaks of 101 and single-sided oxides. The Raman shift corresponding to the 101 content was 800-900 cm⁻¹. -1 The Raman shift corresponding to the single-sided oxide content is 750-800 cm⁻¹. -1 The peak areas of the corresponding characteristic peaks were calculated, and the Raman content of 101 and the single-sided oxide (5-tert-butylperoxide-2,5-dimethylhexane-2-ylhydroperoxide, which is 2,5-dimethyl-2,5-disperoxide hexane with tert-butyl substitution for the single hydrogen atom) were calculated. Regression relationships were established between these values ​​and the chromatographic content. The regression equation between the Raman content of 101 and the chromatographic content was y = 0.9875 + 1.118x, and the regression equation between the Raman content of the single-sided oxide and the chromatographic content was y = 0.9980 - 0.0505x. Figure 3 and Figure 4 , Figure 3 and Figure 4 The discrete data on the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane and its single-sided oxide are respectively derived from... Figure 3 and Figure 4 It can be seen that the discrete data is relatively good, the model relationship is relatively stable, the content data is accurate, and the deviation value is small, so this model can be used for detection and analysis. The goodness of fit R101 is... 2 The goodness of fit R for the unilateral oxide is 0.991. 2The goodness of fit is 0.992, indicating a high level of fit and a small modeling error. The obtained peak area is correlated with the peak area obtained by gas chromatography to determine their functional relationship. This allows for the correction and optimization of the Raman spectral model. For points with large deviations, the sampling rate is increased and these points are subtracted before refitting. The corrected Raman spectral model is as follows:

[0034] Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. Indicates the spectral fitting region. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. 101 gas chromatographic data were obtained according to T / CPCIF 0021-2018 "Industrial grade 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane".

[0035] The detection conditions using the Raman spectrometer were: integration time of 8000 ms, number of sampling points of 4, and number of dark spectrum acquisitions of 1. Each sample was scanned 5 times using the Raman spectrometer.

[0036] Example 2 The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy includes the following steps: Online continuous monitoring is performed using the Raman spectroscopy model established in Example 1. During the material stirring reaction in the reactor, a portion of the material is pumped out to the oil-water separator for automatic separation. Due to the different densities of oil and water, the crude oil phase material 101 flows back into the reactor through the upper oil phase overflow pipe, while the lower aqueous phase material, the synthesis mother liquor, returns to the reactor through the aqueous phase balance pipe. The gas phase balance pipe balances the gas pressure in the pipeline and the oil-water separator, ensuring stable system operation. The bottom valve ensures unidirectional flow of the aqueous phase into the aqueous phase balance pipe, preventing backflow and ensuring stable operation of the entire system. The Raman spectroscopy online detector probe extends from the top of the oil-water separator into the crude oil phase material 101. Using the Raman spectroscopy model established in Example 1, online continuous monitoring is performed. The Raman spectrometer is set to work continuously, automatically starting the second detection after the first detection is completed. Each detection takes 150 seconds. The reaction system is continuously monitored during the reaction process, and the detection results are obtained in real time.

[0037] The Raman spectroscopy was set to continuous operation with an initial integration time of 2000 ms, 6 sampling points, and 2 dark spectrum acquisitions. The next detection began after each data acquisition was completed. Subsequently, the integration time was increased by 1000 ms every 15 minutes until the reaction endpoint was reached. Each sample was scanned 5 times using a Raman spectrometer.

[0038] Samples were taken every 15 minutes during the reaction and analyzed using a gas chromatograph as comparative data.

[0039] The detection data obtained by the two detection methods are shown in Tables 5 and 6. Analysis of the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content during the reaction showed a maximum difference of 0.14% and an average difference of 0.07%. Analysis of the single-sided oxides during the reaction showed a maximum difference of 0.20% and an average difference of 0.08%. The data accuracy is high.

[0040] Table 5. Detection values ​​of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content.

[0041] Table 6. Detection values ​​of unilateral oxide content

[0042] Example 3 The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy includes the following steps: Online continuous monitoring is performed using the Raman spectroscopy model established in Example 1. During the material stirring reaction in the reactor, a portion of the material is pumped out to the oil-water separator for automatic separation. Due to the different densities of oil and water, the crude oil phase material 101 flows back into the reactor through the upper oil phase overflow pipe, while the lower aqueous phase material, the synthesis mother liquor, returns to the reactor through the aqueous phase balance pipe. The gas phase balance pipe balances the gas pressure in the pipeline and the oil-water separator, ensuring stable system operation. The bottom valve ensures unidirectional flow of the aqueous phase into the aqueous phase balance pipe, preventing backflow and ensuring stable operation of the entire system. The Raman spectroscopy online detector probe extends from the top of the oil-water separator into the crude oil phase material 101. Using the Raman spectroscopy model established in Example 1, online continuous monitoring is performed. The Raman spectrometer is set to work continuously, automatically starting the second detection after the first detection is completed. Each detection takes 180 seconds. The reaction system is continuously monitored during the reaction process, and the detection results are obtained in real time.

[0043] The Raman spectroscopy was set to continuous operation with an initial integration time of 1500 ms, 8 sampling points, and 3 dark spectrum acquisitions. The next detection began after each data acquisition was completed. Subsequently, the integration time was increased by 1500 ms every 20 minutes until the reaction endpoint was reached. Each sample was scanned 4 times using a Raman spectrometer.

[0044] Samples were taken every 15 minutes during the reaction and analyzed using a gas chromatograph as comparative data.

[0045] The detection data obtained by the two detection methods are shown in Tables 7 and 8. Analysis of the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content during the reaction showed a maximum difference of 0.24% and an average difference of 0.19%. Analysis of the single-sided oxides during the reaction showed a maximum difference of 0.16% and an average difference of 0.08%. The data accuracy is high.

[0046] Table 7. Detection values ​​of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content.

[0047] Table 8. Detection values ​​of unilateral oxide content

[0048] Example 4 The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy includes the following steps: Online continuous monitoring is performed using the Raman spectroscopy model established in Example 1. During the material stirring reaction in the reactor, a portion of the material is pumped out to the oil-water separator for automatic separation. Due to the different densities of oil and water, the crude oil phase material 101 flows back into the reactor through the upper oil phase overflow pipe, while the lower aqueous phase material, the synthesis mother liquor, returns to the reactor through the aqueous phase balance pipe. The gas phase balance pipe balances the gas pressure in the pipeline and the oil-water separator, ensuring stable system operation. The bottom valve ensures unidirectional flow of the aqueous phase into the aqueous phase balance pipe, preventing backflow and ensuring stable operation of the entire system. The Raman spectroscopy online detector probe extends from the top of the oil-water separator into the crude oil phase material 101. Using the Raman spectroscopy model established in Example 1, online continuous monitoring is performed. The Raman spectrometer is set to work continuously, automatically starting the second detection after the first detection is completed. Each detection takes 120 seconds. The reaction system is continuously monitored during the reaction process, and the detection results are obtained in real time.

[0049] The Raman spectroscopy was set to continuous operation with an initial integration time of 1000 ms, 4 sampling points, and 1 dark spectrum acquisition. The next detection began after each data acquisition was completed. Subsequently, the integration time was increased by 800 ms every 10 minutes until the reaction endpoint was reached. The number of scans for each sample was determined using a Raman spectrometer (3 scans).

[0050] Samples were taken every 15 minutes during the reaction and analyzed using a gas chromatograph as comparative data.

[0051] The detection data obtained by the two detection methods are shown in Tables 9 and 10. Analysis of the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content during the reaction showed a maximum difference of 0.30% and an average difference of 0.15%. Analysis of the single-sided oxides during the reaction showed a maximum difference of 0.17% and an average difference of 0.11%. The data accuracy is high.

[0052] Table 9. Detection values ​​of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content.

[0053] Table 10 Detection values ​​of unilateral oxide content

[0054] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any modifications and substitutions based on the technical solutions and inventive concepts provided by the present invention should be covered within the scope of protection of the present invention.

Claims

1. A method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy, characterized in that, Includes the following steps: (1) Raman spectra of n 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with known content data were determined by Raman spectrometer. (2) The 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane samples with n known content data from step (1) were determined by gas chromatography and chemical analysis. The gas chromatography data of the n samples with known content data were compared with the Raman spectra of the n samples with known content data obtained in step (1). A model relationship between the two was established using chemometrics software. The model relationship between the two is as follows: Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. This represents the spectral fitting region, and N represents the number of Lorentz peaks. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. (3) Use a Raman spectrometer to determine the content data of n samples to be tested. According to the model relationship in step (2), obtain the content data of n samples to be tested. Then use gas chromatography and chemical analysis to determine the content data of n samples to be tested. Compare the gas chromatography data of the n samples to be tested with the content data of the n samples to be tested obtained according to the model relationship in step (2). Perform adaptive baseline subtraction on the Raman spectrum of the sample to be tested to correct it. Perform Lorentz peak fitting and peak separation on the corrected Raman spectrum to extract the characteristic peaks of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane and the single-sided oxide 5-tert-butylperoxide-2,5-dimethylhexane-2-ylhydrogen peroxide. Calculate the peak area of ​​the corresponding characteristic peak. Correlate the obtained peak area with the peak area obtained by gas chromatography to find its functional relationship. Correct and optimize the Raman spectral model. For points with large deviations, increase the sampling amount and subtract points with large deviations. Refit. The corrected Raman spectral model is: Where J represents the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in the sample to be tested in wt%, and v represents the wavenumber. The normalized measured spectrum of the sample is shown below. Indicates the spectral fitting region. These represent the peak area, center position, and half-width at half-maximum of the peak, respectively. (4) During the stirring reaction of materials in the reactor, some materials are collected by diaphragm pump and automatically separated in oil-water separator. Due to the different densities of oil and water, the crude oil phase material 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane flows back into the reactor through the upper oil phase overflow pipe, while the lower water phase material synthesis mother liquor returns to the reactor through the water phase balance pipe. The Raman spectrometer detection probe extends from the upper end of the oil-water separator into the crude oil phase material 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane and uses the Raman spectroscopy model established in step (3) for online continuous monitoring. In steps (1)-(3), n≥20.

2. The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy according to claim 1, characterized in that, In step (1), the 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane sample with known content data has a 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane content of 60-85% and a single-sided oxide content of 0-20%.

3. The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy according to claim 1, characterized in that, In steps (2) and (3), the gas chromatographic data of 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane were determined according to T / CPCIF 0021-2018 "Industrial 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane".

4. The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy according to claim 1, characterized in that, In steps (1) and (3)-(4), the detection conditions of the Raman spectrometer are: integration time of 1000-20000ms, number of sampling points of 3-8, and number of dark spectrum acquisitions of 1-3.

5. The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy according to claim 1, characterized in that, In steps (1) and (3)-(4), the number of scans for each sample is not less than 3 using a Raman spectrometer.

6. The method for analyzing the content of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane based on Raman spectroscopy according to claim 1, characterized in that, In step (4), the Raman spectrometer is set to work continuously. After one detection is completed, the second detection will start automatically. Each detection takes 4-220 seconds. The reaction system is continuously detected during the reaction process and the detection results are obtained in real time.

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