System and method for detecting impurities in bis (tert-butylperoxy) diisopropyl benzene

Abstract

The invention provides a system and a method for detecting impurities in bis (tert-butylperoxy) diisopropyl benzene, the system comprises a detection cavity, an inert gas purging pipeline, a microfluidic sampling device, a spectrum detection module, a micro chromatography-mass spectrometry module and a control and data processing module, through the modules, real-time monitoring and early warning are realized, the detection safety is improved, and the detection accuracy is improved. Results are fed back in real time in each step of sample collection, spectrum preliminary screening and mass spectrometry, any detected abnormal data can immediately trigger a control signal through real-time monitoring, and potential risks caused by accumulation of peroxide or other harmful impurities in the production process are effectively avoided. The spectrum detection module and the micro chromatography-mass spectrometry module are combined, efficient cooperation is achieved in the detection process, the detection time is shortened to the maximum extent, inert gas protection is conducted through the inert gas purging pipeline, decomposition or reaction of peroxide in bis (tert-butylperoxy) diisopropyl benzene is avoided, and higher safety guarantee is provided for detection.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical analysis and detection, and more specifically, to a system and method for detecting impurities in di-tert-butyl diisopropyl peroxide. Background Art

[0002] Diisopropyl di-tert-butyl peroxide (DBP-DIPB) is a common organic peroxide with high initiation activity and low decomposition temperature. It is often used in polymerization, cross-linking and vulcanization. However, DBP-DIPB is prone to produce a variety of by-products or impurities (such as other peroxide derivatives, oxidation by-products, etc.) during the synthesis or storage and transportation process.

[0003] At present, the detection of impurity content in diisopropylbenzene ditert-butyl peroxide generally adopts offline analysis methods, such as gas chromatography-mass spectrometry (GC-MS) or high performance liquid chromatography (HPLC). However, these offline detection methods often have shortcomings such as cumbersome sampling, long time consumption, inability to monitor in real time, and high requirements for operating environment and personnel. At the same time, when handling potentially dangerous peroxides, if there are no perfect safety protection measures, there may also be safety risks.

[0004] In view of this, the present invention proposes a system and method for detecting impurities in diisopropylbenzene di-tert-butyl peroxide, which can realize rapid detection under the protection of inert gas and has high sensitivity and automation. Summary of the invention

[0005] The purpose of the present invention is to provide a system and method for detecting impurities in di-tert-butyl diisopropylbenzene peroxide, which can realize rapid detection under the protection of inert gas and has high sensitivity and automation.

[0006] A detection system for impurities in di-tert-butyl diisopropylbenzene peroxide comprises a detection cavity, an inert gas purge pipeline, a microfluidic sampling device, a spectrum detection module, a micro-chromatography mass spectrometry module, a control and data processing module, and a cleaning module, wherein the sampling port of a di-tert-butyl diisopropylbenzene peroxide material storage device is connected to an input end of a detection cavity module through a microfluidic sampling device, the microfluidic sampling device is used to control the injection rate of the di-tert-butyl diisopropylbenzene peroxide material, the output end of the detection cavity module is connected to an external waste recovery device, the detection cavity has a corrosion-resistant lining, a safety explosion-proof module and a temperature control module are arranged in the detection cavity, the detection cavity is used to receive detection samples of the di-tert-butyl diisopropylbenzene peroxide material storage device and perform temperature control and inert gas insulation on the samples, inert gas purge pipelines are arranged at the input end and the output end of the detection cavity module, and the inert gas purge pipeline is connected to the detection cavity The inert gas purge pipeline is used to maintain the inert environment inside the detection chamber. The detection chamber is connected with a spectral detection module and a micro-chromatography-mass spectrometry module. The spectral detection module is used to quickly detect the characteristic peaks of peroxide groups or aromatic groups in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The micro-chromatography-mass spectrometry module is used to finely separate and mass spectrometrically analyze the impurities in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The inert gas purge pipeline and the detection chamber module are both connected with a cleaning module. The cleaning module is used to clean and purge to ensure the quality of the detection environment. The control and data processing module is connected with the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module through signals. The control and data processing module is used to control the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module.

[0007] In some embodiments, the microfluidic injection device includes a micro pump, a mass flow meter, and a micro valve, which can accurately control the injection volume and rate of the DBP-DIPB sample. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device enters the detection cavity module in sequence through the micro pump, the mass flow meter, and the micro valve. The micro pump is one of a corrosion-resistant micro diaphragm pump or a plunger pump.

[0008] In some embodiments, the spectral detection module is a mid-infrared spectrometer, the detection wavenumber range covers the peroxide characteristic region of 3000 to 3500 cm^-1, and the spectral threshold is set to 1.0 Abs.

[0009] In some embodiments, the micro chromatography mass spectrometry module is a Micro GC-TOF-MS and is equipped with a capillary chromatography column with programmable temperature.

[0010] In some embodiments, the control and data processing module is connected to a preset database, which is used to compare the characteristic spectrum or mass spectrum fingerprint of impurities and automatically alarm.

[0011] A method for detecting impurities in diisopropyl di-tert-butyl peroxide, characterized in that it comprises the following steps:

[0012] Step 1: Sample collection and pretreatment, the sample is output from the sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device and output to the detection cavity through the microfluidic injection device, wherein the injection flow rate is 100-200 μL / min, and the injection volume is 50-200 μL;

[0013] Step 2: The sample enters the detection chamber and is purged and temperature controlled. After the sample enters the detection chamber, the inert gas purge pipeline is continuously purged to prevent oxygen from reacting with the sample. At the same time, the temperature control module controls the chamber temperature to 40°C-50°C to ensure that no peroxy decomposition occurs and the spectral data is stable. The purge time of the inert gas purge pipeline is 3-5 minutes, and the purge flow rate is 2L / min.

[0014] Step 3: The sample is preliminarily screened by the spectrum detection module to obtain spectrum data. The sample is irradiated by the light source in the monitoring cavity. The spectrum monitoring module scans the sample to detect the characteristic absorption peaks of the peroxide group and the aromatic ring group in the sample and obtains the spectrum data. When the spectrum data is lower than the preset threshold, the process proceeds to step 6. If the spectrum data is higher than the preset threshold, the process proceeds to step 4.

[0015] Step 4: The sample is subjected to mass spectrometry analysis by a micro-chromatography mass spectrometry module to obtain mass spectrum data. When the spectrum data is higher than a preset threshold, step 4 is entered to perform fine separation and mass number detection to obtain mass spectrum data, and the mass spectrum data is compared with the database to determine the type and content of impurities in the sample. If the impurities in the sample cannot be determined, then the impurities are unknown impurities, and an alarm is issued through the control and data processing module to shut down. If the impurity content is lower than the preset threshold, the system will operate normally. If the impurity content exceeds the preset threshold, an alarm is issued through the control and data processing module to shut down.

[0016] Step 5: The control and data processing module collects spectral data and mass spectrometry data in real time to dynamically adjust the sample detection standard. The control and data processing module uses a dynamic threshold adjustment algorithm to collect historical data and analyze the parameters of real-time samples, automatically optimize the dynamic threshold, dynamically adjust the sensitivity of impurity identification, and reduce false positives and false negatives;

[0017] Step 6: Automatic cleaning and preparation for the next test. After completing the above steps, the control and data processing module starts the cleaning program and uses inert gas or solvent to clean the detection cavity and inert gas purge pipeline to ensure that no impurities remain.

[0018] In some embodiments, step four also includes: mass spectrometry analysis to obtain mass spectrum data. When the spectrum data is higher than a preset threshold, step four is entered, the sample is separated by micro gas chromatography, and then the sample molecules are ionized by an electron bombardment ion source, and the charged ions are sent to a mass spectrometer, and the mass spectrum of each ion is obtained by analyzing its mass-to-charge ratio (m / z). Each peak corresponds to a specific ion, and the collected mass spectrum data is compared with a preset standard impurity library to identify the type of impurities in the sample, and the concentration of the impurity is calculated by quantitative analysis based on the area or height of the peak. If it cannot be determined, the impurity in the sample is an unknown impurity, and an alarm is issued and shut down through the control and data processing module. If the impurity content is lower than the preset threshold, normal operation is performed. If the impurity content exceeds the preset threshold, an alarm is issued and shut down through the control and data processing module.

[0019] In some embodiments, the absorption peak threshold of the spectrum detection module is set to 1.0 Abs, and when the peak value exceeds the threshold, the mass spectrometry detection process is automatically entered.

[0020] In some embodiments, step four also includes that in the micro-chromatography mass spectrometry module, the chromatographic column is a DB-5 capillary chromatographic column, the temperature program is an initial temperature of 40°C, the initial temperature stage is maintained for 2 minutes, and then the temperature is increased at a rate of 10-15°C / min until the final temperature reaches 200°C, and the final temperature stage is maintained for 5 minutes.

[0021] In some embodiments, step four also includes, in the micro-chromatography mass spectrometry module, the mass-to-charge ratio (m / z) range is 50-500Da, and the data acquisition frequency is 1000 data points per second.

[0022] In some embodiments, step six also includes continuously purging with nitrogen or argon at a flow rate of 2 L / min for 3-5 minutes, and flushing with an organic solvent to ensure that there is no residue in the system.

[0023] In some embodiments, step five also includes that the dynamic threshold calculation formula in the dynamic threshold adjustment algorithm is: dynamic threshold = basic threshold * (1 + α * ΔT)), ΔT represents the difference between the parameters of the sample and the standard setting parameters, α is the sensitivity adjustment, and therefore represents the degree of influence of the environmental parameters on the threshold. For example, the basic threshold is 1.0Abs, ΔT = ±5°C, α is 0.02, then it is calculated that the dynamic threshold = 1.0*(1+0.02*5) = 1.1.

[0024] The beneficial effects of the present invention are as follows: the present invention proposes a system and method for detecting impurities in di-tert-butyl diisopropylbenzene peroxide, comprising a detection chamber, an inert gas purge pipeline, a microfluidic sampling device, a spectral detection module, a micro-chromatography mass spectrometry module, and a control and data processing module. The modules are used to realize real-time monitoring and early warning, improve detection safety, and provide real-time feedback on results in each step of sample collection, spectral screening, and mass spectrometry analysis. Through real-time monitoring, any abnormal data detected can immediately trigger a control signal, effectively avoiding potential dangers caused by accumulation of peroxides or other harmful impurities in the production process. By combining the spectral detection module and the micro-chromatography mass spectrometry module, efficient collaboration is achieved during the detection process, reducing the detection time to the greatest extent, and inert gas protection is performed through the inert gas purge pipeline, thereby avoiding decomposition or reaction of peroxides in di-tert-butyl diisopropylbenzene peroxide, providing a higher safety guarantee for detection. The control and data processing module automatically adjusts the detection threshold through a dynamic threshold adjustment algorithm under different production environment conditions. The dynamic threshold adjustment ensures that even if changes in environmental parameters such as temperature and flow rate can affect the spectrum and mass spectrometry signals of the sample, the system can still maintain a high sensitivity and avoid missed reports and false alarms. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic structural diagram of an impurity detection system in diisopropyl di-tert-butyl peroxide of the present application.

[0026] Figure 2 The present invention is a schematic flow chart of a method for detecting impurities in diisopropyl di-tert-butyl peroxide of the present invention.

[0027] Main component symbols

[0028] The following specific implementation manner will further illustrate the present invention in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION

[0029] The following examples are described to assist the understanding of the present application, and the examples are not and should not be interpreted in any way as limiting the scope of protection of the present application.

[0030] In the following description, those skilled in the art will recognize that throughout this discussion, components may be described as separate functional units (which may include sub-units), but those skilled in the art will recognize that various components or portions thereof may be divided into separate components or may be integrated together (including within a single system or component).

[0031] At the same time, the connections between components or systems are not intended to be limited to direct connections, rather, the data between these components may be modified, reformatted, or otherwise changed by intermediate components. In addition, additional or fewer connections may be used. It should also be noted that the terms "coupled," "connected," or "input" should be understood to include direct connections, indirect connections through one or more intermediate devices, and wireless connections.

[0032] Embodiment 1:

[0033] like Figure 1 As shown, it is a structural schematic diagram of an impurity detection system in diisopropyl di-tert-butyl peroxide of the present application; Figure 2 Shown is a schematic flow chart of a method for detecting impurities in diisopropyl di-tert-butyl peroxide of the present application.

[0034] A detection system for impurities in di-tert-butyl diisopropylbenzene peroxide comprises a detection cavity, an inert gas purge pipeline, a microfluidic sampling device, a spectrum detection module, a micro-chromatography mass spectrometry module, a control and data processing module, and a cleaning module, wherein the sampling port of a di-tert-butyl diisopropylbenzene peroxide material storage device is connected to an input end of a detection cavity module through a microfluidic sampling device, the microfluidic sampling device is used to control the injection rate of the di-tert-butyl diisopropylbenzene peroxide material, the output end of the detection cavity module is connected to an external waste recovery device, the detection cavity has a corrosion-resistant lining, a safety explosion-proof module and a temperature control module are arranged in the detection cavity, the detection cavity is used to receive detection samples of the di-tert-butyl diisopropylbenzene peroxide material storage device and perform temperature control and inert gas insulation on the samples, inert gas purge pipelines are arranged at the input end and the output end of the detection cavity module, and the inert gas purge pipeline is connected to the detection cavity The inert gas purge pipeline is used to maintain the inert environment inside the detection chamber. The detection chamber is connected with a spectral detection module and a micro-chromatography-mass spectrometry module. The spectral detection module is used to quickly detect the characteristic peaks of peroxide groups or aromatic groups in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The micro-chromatography-mass spectrometry module is used to finely separate and mass spectrometrically analyze the impurities in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The inert gas purge pipeline and the detection chamber module are both connected with a cleaning module. The cleaning module is used to clean and purge to ensure the quality of the detection environment. The control and data processing module is connected with the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module through signals. The control and data processing module is used to control the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module.

[0035] The microfluidic injection device includes a micro pump, a mass flow meter, and a micro valve, which can accurately control the injection volume and rate of the DBP-DIPB sample. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device enters the detection cavity module through the micro pump, mass flow meter, and micro valve in sequence. The micro pump is one of the corrosion-resistant micro diaphragm pumps or plunger pumps.

[0036] The spectrum detection module is a mid-infrared spectrometer, the detection wavenumber range covers the peroxide characteristic region of 3100 to 3400 cm^-1, and the spectrum threshold is set to 1.0 Abs.

[0037] The micro-chromatography mass spectrometry module is a Micro GC-TOF-MS and is equipped with a capillary chromatographic column with programmable temperature rise.

[0038] The control and data processing module is connected to a preset database, which is used to compare the characteristic spectrum or mass spectrum fingerprint of impurities and automatically alarm.

[0039] Test conditions:

[0040] The sample volume was 100 μL, the spectral reference threshold was 1.0 Abs, and the wavelength range was 3100 to 3400 cm^-1.

[0041] A method for detecting impurities in di-tert-butyl diisopropylbenzene peroxide comprises the following steps:

[0042] Step 1: Sample collection and pretreatment. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device outputs 100 μL of material and outputs it to the detection cavity through the microfluidic injection device, wherein the injection flow rate is 100-200 μL / min, and the injection volume is 1 μL; Step 2: The sample enters the detection cavity and is purged and temperature controlled. After the sample enters the detection cavity, the inert gas purge pipeline is continuously purged to prevent oxygen from reacting with the sample. At the same time, the temperature control module controls the cavity temperature to 40°C-50°C to ensure that no peroxy decomposition occurs and ensure the stability of the spectral data. Among them, the purge time of the inert gas purge pipeline is 3-5 minutes, and the purge flow rate is 2L / min;

[0043] Step 3: The sample is preliminarily screened by the spectrum detection module to obtain spectrum data. The sample is irradiated by the light source in the monitoring cavity. The spectrum monitoring module scans the sample to detect the characteristic absorption peaks of the peroxide group and the aromatic ring group in the sample and obtains the spectrum data of 1.2Abs. The absorption peak threshold of the spectrum detection module is set to 1.0Abs, and the corresponding impurity content range is about 100ppm. When the peak value exceeds the threshold, enter step 4;

[0044] Step 4: The sample is subjected to mass spectrometry analysis by a micro-chromatography mass spectrometry module to obtain mass spectrometry data. In the micro-chromatography mass spectrometry module, the chromatographic column is a DB-5 capillary chromatographic column, and the temperature program is an initial temperature of 40°C, which is maintained for 2 minutes in the initial temperature stage, followed by heating at a rate of 10-15°C / min until the final temperature reaches 200°C, which is maintained for 5 minutes in the final temperature stage; in the micro-chromatography mass spectrometry module, the mass-to-charge ratio (m / z) range is 50-500Da, and the data acquisition frequency is 1000 data points per second. Fine separation and mass number detection are performed to obtain mass spectrometry data, and the mass spectrometry data is compared with the database to determine the type and content of impurities in the sample. If the impurities in the sample cannot be determined, they are unknown impurities, which are then processed by the control and data processing module. Alarm shutdown. If the impurity content is lower than the preset threshold, it will run normally. If the impurity content exceeds the preset threshold, the control and data processing module will alarm and shut down. Specifically, mass spectrometry analysis obtains mass spectrum data. When the spectrum data is higher than the preset threshold, it enters step 4. The sample is separated by micro gas chromatography, and then the sample molecules are ionized by electron bombardment ion source. The charged ions are sent to the mass spectrometer, and the mass spectrum of each ion is obtained by analyzing its mass-to-charge ratio (m / z). Each peak corresponds to a specific ion, and the mass spectrum m / z value is 150,250. The collected mass spectrum data is compared with the preset standard impurity library to identify the type of impurities in the sample, and the concentration of the impurity is calculated to be 60ppm based on the peak area or height.

[0045] Step 5: The control and data processing module collects spectral data and mass spectrometry data in real time to dynamically adjust the sample detection standard. The control and data processing module uses a dynamic threshold adjustment algorithm to collect historical data and analyze the parameters of real-time samples. The environmental parameters affect the heat exchange of the cavity due to changes in sample flow rate, making ΔT 5°C, the sensitivity adjustment factor is 0.02, and the dynamic threshold adjustment = 1.0*(1+0.02*5) = 1.1Abs

[0046] Step 6: Automatic cleaning and preparation for the next test. After completing the above steps, the control and data processing module starts the cleaning program and uses inert gas or solvent to clean the detection cavity and inert gas purge pipeline to ensure that no impurities remain.

[0047] The following Table 1 is obtained through the above steps:

[0048] Sample sampling volume 100μL Spectral absorbance 1.2Abs Wavelength range 3100~3400cm^-1 Mass spectrum m / z value 150,250 Impurity concentration 60ppm Dynamic threshold adjustment 1.1Abs Baseline Threshold 1.0Abs Threshold setting 100ppm

[0049] From Table 1 and the above content, it can be seen that the spectral absorbance is 1.2Abs, which exceeds the adjusted threshold value (1.1Abs). Although the impurity concentration is 60ppm (within the limit), the machine is not shut down.

[0050] Embodiment 2:

[0051] like Figure 1 As shown, it is a structural schematic diagram of an impurity detection system in diisopropyl di-tert-butyl peroxide of the present application; Figure 2 Shown is a schematic flow chart of a method for detecting impurities in diisopropyl di-tert-butyl peroxide of the present application.

[0052] A detection system for impurities in di-tert-butyl diisopropylbenzene peroxide comprises a detection cavity, an inert gas purge pipeline, a microfluidic sampling device, a spectrum detection module, a micro-chromatography mass spectrometry module, a control and data processing module, and a cleaning module, wherein the sampling port of a di-tert-butyl diisopropylbenzene peroxide material storage device is connected to an input end of a detection cavity module through a microfluidic sampling device, the microfluidic sampling device is used to control the injection rate of the di-tert-butyl diisopropylbenzene peroxide material, the output end of the detection cavity module is connected to an external waste recovery device, the detection cavity has a corrosion-resistant lining, a safety explosion-proof module and a temperature control module are arranged in the detection cavity, the detection cavity is used to receive detection samples of the di-tert-butyl diisopropylbenzene peroxide material storage device and perform temperature control and inert gas insulation on the samples, inert gas purge pipelines are arranged at the input end and the output end of the detection cavity module, and the inert gas purge pipeline is connected to the detection cavity The inert gas purge pipeline is used to maintain the inert environment inside the detection chamber. The detection chamber is connected with a spectral detection module and a micro-chromatography-mass spectrometry module. The spectral detection module is used to quickly detect the characteristic peaks of peroxide groups or aromatic groups in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The micro-chromatography-mass spectrometry module is used to finely separate and mass spectrometrically analyze the impurities in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The inert gas purge pipeline and the detection chamber module are both connected with a cleaning module. The cleaning module is used to clean and purge to ensure the quality of the detection environment. The control and data processing module is connected with the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module through signals. The control and data processing module is used to control the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module.

[0053] The microfluidic injection device includes a micro pump, a mass flow meter, and a micro valve, which can accurately control the injection volume and rate of the DBP-DIPB sample. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device enters the detection cavity module through the micro pump, mass flow meter, and micro valve in sequence. The micro pump is one of the corrosion-resistant micro diaphragm pumps or plunger pumps.

[0054] The spectrum detection module is a mid-infrared spectrometer, the detection wavenumber range covers the peroxide characteristic region of 3100 to 3400 cm^-1, and the spectrum threshold is set to 1.0 Abs.

[0055] The micro-chromatography mass spectrometry module is a Micro GC-TOF-MS and is equipped with a capillary chromatographic column with programmable temperature rise.

[0056] The control and data processing module is connected to a preset database, which is used to compare the characteristic spectrum or mass spectrum fingerprint of impurities and automatically alarm.

[0057] Test conditions:

[0058] The sample volume was 100 μL, the spectral reference threshold was 1.0 Abs, and the wavelength range was 3100 to 3400 cm^-1.

[0059] A method for detecting impurities in di-tert-butyl diisopropylbenzene peroxide comprises the following steps:

[0060] Step 1: Sample collection and pretreatment. The sampling port of the diisopropylbenzene ditert-butyl peroxide material storage device outputs 150 μL of material and outputs it to the detection cavity through the microfluidic injection device, wherein the injection flow rate is 100-200 μL / min, and the injection volume is 1 μL; Step 2: The sample enters the detection cavity and is purged and temperature controlled. After the sample enters the detection cavity, the inert gas purge pipeline is continuously purged to prevent oxygen from reacting with the sample. At the same time, the temperature control module controls the cavity temperature to 40°C-50°C to ensure that no peroxy decomposition occurs and ensure the stability of the spectral data. Among them, the purge time of the inert gas purge pipeline is 3-5 minutes, and the purge flow rate is 2L / min;

[0061] Step 3: The sample is preliminarily screened by the spectrum detection module to obtain spectrum data. The sample is irradiated by the light source in the monitoring cavity. The spectrum monitoring module scans the sample to detect the characteristic absorption peaks of the peroxide group and the aromatic ring group in the sample and obtains the spectrum data of 1.5Abs. The absorption peak threshold of the spectrum detection module is set to 1.0Abs, and the corresponding impurity content range is about 100ppm. When the peak value exceeds the threshold, enter step 4;

[0062] Step 4: The sample is subjected to mass spectrometry analysis by a micro-chromatography mass spectrometry module to obtain mass spectrometry data. In the micro-chromatography mass spectrometry module, the chromatographic column is a DB-5 capillary chromatographic column, and the temperature program is an initial temperature of 40°C, which is maintained for 2 minutes in the initial temperature stage, followed by heating at a rate of 10-15°C / min until the final temperature reaches 200°C, which is maintained for 5 minutes in the final temperature stage; in the micro-chromatography mass spectrometry module, the mass-to-charge ratio (m / z) range is 50-500Da, and the data acquisition frequency is 1000 data points per second. Fine separation and mass number detection are performed to obtain mass spectrometry data, and the mass spectrometry data is compared with the database to determine the type and content of impurities in the sample. If the impurities in the sample cannot be determined, they are unknown impurities, which are then processed by the control and data processing module. Alarm shutdown. If the impurity content is lower than the preset threshold, it will run normally. If the impurity content exceeds the preset threshold, the control and data processing module will alarm and shut down. Specifically, mass spectrometry analysis obtains mass spectrum data. When the spectrum data is higher than the preset threshold, it enters step 4. The sample is separated by micro gas chromatography, and then the sample molecules are ionized by electron bombardment ion source. The charged ions are sent to the mass spectrometer, and the mass spectrum of each ion is obtained by analyzing its mass-to-charge ratio (m / z). Each peak corresponds to a specific ion, and the mass spectrum m / z value is 150,250. The collected mass spectrum data is compared with the preset standard impurity library to identify the type of impurities in the sample, and the concentration of the impurity is calculated to be 110ppm based on the area or height of the peak.

[0063] Step 5: The control and data processing module collects spectral data and mass spectrometry data in real time to dynamically adjust the sample detection standard. The control and data processing module uses a dynamic threshold adjustment algorithm to collect historical data and analyze the parameters of real-time samples. In the environmental parameters, the change in sample flow rate affects the heat exchange of the cavity, making ΔT 10°C, the sensitivity adjustment factor 0.02, and the dynamic threshold adjustment = 1.0*(1+0.02*10) = 1.2Abs

[0064] Step 6: Automatic cleaning and preparation for the next test. After completing the above steps, the control and data processing module starts the cleaning program and uses inert gas or solvent to clean the detection cavity and inert gas purge pipeline to ensure that no impurities remain.

[0065] The following Table 2 is obtained through the above steps:

[0066] Sample sampling volume 150μL Spectral absorbance 1.5Abs Wavelength range 3100~3400cm^-1 Mass spectrum m / z value 150,250 Impurity concentration 110ppm Dynamic threshold adjustment 1.2Abs Baseline Threshold 1.0Abs Threshold setting 100ppm

[0067] From Table 2 and the above content, it can be seen that the spectral absorbance is 1.5Abs, which exceeds the adjusted threshold value (1.2Abs), and the impurity concentration is 110ppm, which exceeds the set 100pm, triggering a shutdown.

[0068] Embodiment 3:

[0069] like Figure 1 As shown, it is a structural schematic diagram of an impurity detection system in diisopropyl di-tert-butyl peroxide of the present application; Figure 2 Shown is a schematic flow chart of a method for detecting impurities in diisopropyl di-tert-butyl peroxide of the present application.

[0070] A detection system for impurities in di-tert-butyl diisopropylbenzene peroxide comprises a detection cavity, an inert gas purge pipeline, a microfluidic sampling device, a spectrum detection module, a micro-chromatography mass spectrometry module, a control and data processing module, and a cleaning module, wherein the sampling port of a di-tert-butyl diisopropylbenzene peroxide material storage device is connected to an input end of a detection cavity module through a microfluidic sampling device, the microfluidic sampling device is used to control the injection rate of the di-tert-butyl diisopropylbenzene peroxide material, the output end of the detection cavity module is connected to an external waste recovery device, the detection cavity has a corrosion-resistant lining, a safety explosion-proof module and a temperature control module are arranged in the detection cavity, the detection cavity is used to receive detection samples of the di-tert-butyl diisopropylbenzene peroxide material storage device and perform temperature control and inert gas insulation on the samples, inert gas purge pipelines are arranged at the input end and the output end of the detection cavity module, and the inert gas purge pipeline is connected to the detection cavity The inert gas purge pipeline is used to maintain the inert environment inside the detection chamber. The detection chamber is connected with a spectral detection module and a micro-chromatography-mass spectrometry module. The spectral detection module is used to quickly detect the characteristic peaks of peroxide groups or aromatic groups in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The micro-chromatography-mass spectrometry module is used to finely separate and mass spectrometrically analyze the impurities in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The inert gas purge pipeline and the detection chamber module are both connected with a cleaning module. The cleaning module is used to clean and purge to ensure the quality of the detection environment. The control and data processing module is connected with the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module through signals. The control and data processing module is used to control the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectral detection module, and the micro-chromatography-mass spectrometry module.

[0071] The microfluidic injection device includes a micro pump, a mass flow meter, and a micro valve, which can accurately control the injection volume and rate of the DBP-DIPB sample. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device enters the detection cavity module through the micro pump, mass flow meter, and micro valve in sequence. The micro pump is one of the corrosion-resistant micro diaphragm pumps or plunger pumps.

[0072] The spectrum detection module is a mid-infrared spectrometer, the detection wavenumber range covers the peroxide characteristic region of 3100 to 3400 cm^-1, and the spectrum threshold is set to 2.0 Abs.

[0073] The micro-chromatography mass spectrometry module is a Micro GC-TOF-MS and is equipped with a capillary chromatographic column with programmable temperature rise.

[0074] The control and data processing module is connected to a preset database, which is used to compare the characteristic spectrum or mass spectrum fingerprint of impurities and automatically alarm.

[0075] Test conditions:

[0076] The sample volume was 200 μL, the spectral reference threshold was 0.9 Abs, and the wavelength range was 3100 to 3400 cm^-1.

[0077] A method for detecting impurities in di-tert-butyl diisopropylbenzene peroxide comprises the following steps:

[0078] Step 1: Sample collection and pretreatment. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device outputs 200 μL of material and outputs it to the detection cavity through the microfluidic injection device, wherein the injection flow rate is 100-200 μL / min, and the injection volume is 1 μL; Step 2: The sample enters the detection cavity and is purged and temperature controlled. After the sample enters the detection cavity, the inert gas purge pipeline is continuously purged to prevent oxygen from reacting with the sample. At the same time, the temperature control module controls the cavity temperature to 40°C-50°C to ensure that no peroxy decomposition occurs and to ensure the stability of the spectral data. Among them, the purge time of the inert gas purge pipeline is 3-5 minutes, and the purge flow rate is 2L / min;

[0079] Step 3: The sample is preliminarily screened by the spectrum detection module to obtain spectrum data. The sample is irradiated by the light source in the monitoring cavity. The spectrum monitoring module scans the sample to detect the characteristic absorption peaks of the peroxide group and the aromatic ring group in the sample and obtains the spectrum data of 2.0Abs. The absorption peak threshold of the spectrum detection module is set to 1.0Abs, and the corresponding impurity content range is about 100ppm. When the peak value exceeds the threshold, enter step 4;

[0080] Step 4: The sample is subjected to mass spectrometry analysis by a micro-chromatography mass spectrometry module to obtain mass spectrometry data. In the micro-chromatography mass spectrometry module, the chromatographic column is a DB-5 capillary chromatographic column, and the temperature program is an initial temperature of 40°C, which is maintained for 2 minutes in the initial temperature stage, followed by heating at a rate of 10-15°C / min until the final temperature reaches 200°C, which is maintained for 5 minutes in the final temperature stage; in the micro-chromatography mass spectrometry module, the mass-to-charge ratio (m / z) range is 50-500Da, and the data acquisition frequency is 1000 data points per second. Fine separation and mass number detection are performed to obtain mass spectrometry data, and the mass spectrometry data is compared with the database to determine the type and content of impurities in the sample. If the impurities in the sample cannot be determined, they are unknown impurities, which are then processed by the control and data processing module. Alarm shutdown. If the impurity content is lower than the preset threshold, it will run normally. If the impurity content exceeds the preset threshold, the control and data processing module will alarm and shut down. Specifically, mass spectrometry analysis obtains mass spectrum data. When the spectrum data is higher than the preset threshold, it enters step 4. The sample is separated by micro gas chromatography, and then the sample molecules are ionized by electron bombardment ion source. The charged ions are sent to the mass spectrometer, and the mass spectrum of each ion is obtained by analyzing its mass-to-charge ratio (m / z). Each peak corresponds to a specific ion, and the mass spectrum m / z value is 150,250. The collected mass spectrum data is compared with the preset standard impurity library to identify the type of impurities in the sample, and the concentration of the impurity is calculated to be 130ppm based on the peak area or height.

[0081] Step 5: The control and data processing module collects spectral data and mass spectrometry data in real time to dynamically adjust the sample detection standard. The control and data processing module uses a dynamic threshold adjustment algorithm to collect historical data and analyze the parameters of real-time samples.

[0082] In the environmental parameters, the change of sample flow rate affects the heat exchange of the cavity, making ΔT 15°C, the sensitivity adjustment factor 0.02, and the dynamic threshold adjustment = 1.0*(1+0.02*15) = 1.3Abs

[0083] Step 6: Automatic cleaning and preparation for the next test. After completing the above steps, the control and data processing module starts the cleaning program and uses inert gas or solvent to clean the detection cavity and inert gas purge pipeline to ensure that no impurities remain.

[0084] The following Table 3 is obtained through the above steps:

[0085] Sample sampling volume 100μL Spectral absorbance 2.0Abs Wavelength range 3100~3400cm^-1 Mass spectrum m / z value 150,250 Impurity concentration 130ppm Dynamic threshold adjustment 1.3Abs Baseline Threshold 1.0Abs Threshold setting 100ppm

[0086] From Table 3 and the above content, it can be seen that the spectral absorbance is 2.0Abs, which exceeds the adjusted threshold value (1.3Abs), and the impurity concentration is 130ppm, which exceeds the set 100pm, triggering a shutdown.

[0087] Although the present application has disclosed multiple aspects and embodiments, other aspects and embodiments will be obvious to those skilled in the art, and several modifications and improvements may be made without departing from the concept of the present application, all of which belong to the protection scope of the present application. The multiple aspects and embodiments disclosed in the present application are only for illustration and are not intended to limit the present application. The actual protection scope of the present application shall be subject to the claims.

Claims

1. A system for detecting impurities in diisopropylbenzene ditert-butylperoxide, comprising a detection chamber, an inert gas purge pipeline, a microfluidic injection device, a spectrum detection module, a micro-chromatography mass spectrometry module, a control and data processing module, and a cleaning module. Features: The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage equipment is connected to the input end of the detection chamber module through a microfluidic injection device, the microfluidic injection device is used to control the injection rate of the di-tert-butyl peroxide diisopropylbenzene material, the output end of the detection chamber module is connected to the external waste recovery equipment, the detection chamber has a corrosion-resistant lining, and a safety explosion-proof module and a temperature control module are arranged in the detection chamber. The detection chamber is used to receive the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment and perform temperature control and insulate the same with inert gas. Inert gas purge pipelines are arranged at the input and output ends of the detection chamber module, the inert gas purge pipelines are connected to the detection chamber, and the inert gas purge pipelines are used to maintain the inert environment inside the detection chamber. The detection chamber is connected with a spectral detection module and a micro-chromatographic The spectrum detection module is used for quickly detecting the characteristic peaks of peroxide groups or aromatic groups in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The micro-chromatography mass spectrometry module is used for fine separation and mass spectrometry analysis of impurities in the detection samples of the di-tert-butyl peroxide diisopropylbenzene material storage equipment. The inert gas purge pipeline and the detection chamber module are both connected with a cleaning module. The cleaning module is used for cleaning and flushing to ensure the quality of the detection environment. The control and data processing module is connected to the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectrum detection module, and the micro-chromatography mass spectrometry module through signals. The control and data processing module is used to control the detection chamber, the inert gas purge pipeline, the microfluidic sampling device, the spectrum detection module, and the micro-chromatography mass spectrometry module.

2. The impurity detection system in diisopropylbenzene ditert-butyl peroxide according to claim 1, characterized in that: The microfluidic injection device includes a micro pump, a mass flow meter, and a micro valve, which can accurately control the injection volume and rate of the DBP-DIPB sample. The sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device enters the detection cavity module through the micro pump, mass flow meter, and micro valve in sequence. The micro pump is one of the corrosion-resistant micro diaphragm pumps or plunger pumps.

3. The impurity detection system in diisopropylbenzene ditert-butyl peroxide according to claim 1, characterized in that: The spectrum detection module is a mid-infrared spectrometer, the detection wavenumber range covers the peroxide characteristic region of 3000 to 3500 cm^-1, and the spectrum threshold is set to 1.0 Abs.

4. The impurity detection system in diisopropyl di-tert-butyl peroxide as claimed in claim 1, characterized in that: The micro-chromatography mass spectrometry module is a Micro GC-TOF-MS and is equipped with a capillary chromatographic column with programmable temperature rise.

5. The impurity detection system in diisopropyl di-tert-butyl peroxide as claimed in claim 1, characterized in that: The control and data processing module is connected to a preset database, which is used to compare the characteristic spectrum or mass spectrum fingerprint of impurities and automatically alarm.

6. A method for detecting impurities in diisopropylbenzene ditert-butylperoxide using the system according to any one of claims 1 to 5, It is characterized in that The following steps are involved: Step 1: Sample collection and pretreatment, the sample is output from the sampling port of the di-tert-butyl peroxide diisopropylbenzene material storage device and output to the detection cavity through the microfluidic injection device, wherein the injection flow rate is 100-200 μL / min, and the injection volume is 50-200 μL; Step 2: The sample enters the detection chamber and is purged and temperature controlled. After the sample enters the detection chamber, the inert gas purge pipeline is continuously purged to prevent oxygen from reacting with the sample. At the same time, the temperature control module controls the chamber temperature to 40°C-50°C to ensure that no peroxy decomposition occurs and the spectral data is stable. The purge time of the inert gas purge pipeline is 3-5 minutes, and the purge flow rate is 2L / min. Step 3: The sample is preliminarily screened by the spectrum detection module to obtain spectrum data. The sample is irradiated by the light source in the monitoring cavity. The spectrum monitoring module scans the sample to detect the characteristic absorption peaks of the peroxide group and the aromatic ring group in the sample and obtains the spectrum data. When the spectrum data is lower than the preset threshold, the process proceeds to step 6. If the spectrum data is higher than the preset threshold, the process proceeds to step 4. Step 4: The sample is subjected to mass spectrometry analysis by a micro-chromatography mass spectrometry module to obtain mass spectrum data. When the spectrum data is higher than a preset threshold, step 4 is entered to perform fine separation and mass number detection to obtain mass spectrum data, and the mass spectrum data is compared with the database to determine the type and content of impurities in the sample. If the impurities in the sample cannot be determined, then the impurities are unknown impurities, and an alarm is issued through the control and data processing module to shut down. If the impurity content is lower than the preset threshold, the system will operate normally. If the impurity content exceeds the preset threshold, an alarm is issued through the control and data processing module to shut down. Step 5: The control and data processing module collects spectral data and mass spectrometry data in real time to dynamically adjust the sample detection standard. The control and data processing module uses a dynamic threshold adjustment algorithm to collect historical data and analyze the parameters of real-time samples, automatically optimize the judgment threshold, dynamically adjust the sensitivity of impurity identification, and reduce false positives and false negatives; Step 6: Automatic cleaning and preparation for the next test. After completing the above steps, the control and data processing module starts the cleaning program and uses inert gas or solvent to clean the detection cavity and inert gas purge pipeline to ensure that no impurities remain.

7. The method for detecting impurities in diisopropyl di-tert-butyl peroxide according to claim 6, wherein: Step four also includes: mass spectrometry analysis to obtain mass spectrum data. When the spectrum data is higher than a preset threshold, step four is entered, the sample is separated by micro gas chromatography, and then the sample molecules are ionized by an electron bombardment ion source, and the charged ions are sent to a mass spectrometer. The mass spectrum of each ion is obtained by analyzing its mass-to-charge ratio (m / z). Each peak corresponds to a specific ion. The collected mass spectrum data is compared with a preset standard impurity library to identify the type of impurities in the sample, and the concentration of the impurities is calculated by quantitative analysis based on the area or height of the peak. If it cannot be determined, the impurities in the sample are unknown impurities, and an alarm is issued and shut down through the control and data processing module. If the impurity content is lower than the preset threshold, normal operation is performed. If the impurity content exceeds the preset threshold, an alarm is issued and shut down through the control and data processing module.

8. The method for detecting impurities in diisopropyl di-tert-butyl peroxide according to claim 6, wherein: Step four also includes that in the micro-chromatography mass spectrometry module, the chromatographic column is a DB-5 capillary chromatographic column, the temperature program is an initial temperature of 40°C, the initial temperature stage is maintained for 2 minutes, and then the temperature is increased at a rate of 10-15°C / min until the final temperature reaches 200°C, and the final temperature stage is maintained for 5 minutes.

9. The method for detecting impurities in diisopropyl di-tert-butyl peroxide according to claim 6, wherein: Step five also includes that the dynamic threshold calculation formula in the dynamic threshold adjustment algorithm is: dynamic threshold = basic threshold * (1 + α * ΔT)), ΔT represents the difference between the sample parameters and the standard setting parameters, and α is the sensitivity adjustment, therefore, it represents the degree of influence of environmental parameters on the threshold.

10. The method for detecting impurities in diisopropyl di-tert-butyl peroxide according to claim 6, characterized in that: Step six also includes continuously purging with nitrogen or argon at a flow rate of 2 L / min for 3-5 minutes, and flushing with an organic solvent to ensure that there is no residue in the system.

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