A method for quickly determining compatibility of chemicals based on raman spectrum

Abstract

The present application relates to the technical field of chemical hazard assessment in petrochemical industry, and discloses a method for rapidly determining compatibility of chemicals based on Raman spectrum. The method comprises the following steps: collecting original spectra of n kinds of chemicals, and storing Raman shift and intensity signals in a spectrometer; preprocessing the original spectra; inputting the preprocessed Raman shift and intensity signals into spectrum characteristic signal analysis software to determine characteristic peak positions and corresponding Raman shift values; substituting the Raman shift values corresponding to the characteristic peak positions into a Raman characteristic peak and active group correlation database to obtain active groups; inputting the active group information into reaction group analysis software to obtain reaction group information; inputting the reaction group information into reactivity analysis software; comparing the reaction group information with reaction groups in a reaction group reaction matrix; and feeding back reaction hazard information. The method can rapidly determine the mixing reaction hazard between unknown chemicals, and provides technical guidance for avoiding hazards.

Description

Technical Field

[0001] This invention relates to the field of chemical hazard assessment technology in the petrochemical industry, specifically to a method for rapidly determining chemical compatibility based on Raman spectroscopy. Background Technology

[0002] In the petrochemical industry, the production, storage, and transportation of chemicals often require mixed storage or formulation. In special circumstances, chemical leaks can inevitably lead to chemical mixing. Chemical compatibility refers to whether a chemical reaction will occur when two or more chemicals are mixed. To mitigate the risks of chemical mixing or reactions, compatibility assessments must be performed before production, storage, and transportation.

[0003] Existing methods for determining chemical compatibility primarily rely on testing, which carries inherent risks and involves relatively complex procedures. Limited by the number of personnel and equipment available, it is difficult to quickly determine chemical compatibility. Currently, the main standards referenced for chemical compatibility testing include: GJB5891.12-2006 Test Methods for Pyrotechnic Agents Part 12: Vacuum Stability Test - Pressure Sensor Method; GJB5891.15-2006 Test Methods for Pyrotechnic Agents Part 15: Compatibility Test - Microcalorimetry; and GJB5891.17-2006 Test Methods for Pyrotechnic Agents Part 17: Compatibility Test - Differential Thermal Analysis and Differential Scanning Calorimetry. These standards primarily determine chemical compatibility by testing the change in gas volume or the exothermic behavior after mixing. CN103983796A "Methods for Testing the Compatibility of Chemicals", CN102680354A "Methods and Applications for Determining the Compatibility of Chemicals", and CN103969289A "Methods for Testing the Compatibility of Chemicals by Microcalorimetry" are similar in principle to the above-mentioned testing standards. They use different testing methods to test the change in gas volume or the exothermic behavior of chemical mixtures to determine whether the chemicals are compatible.

[0004] Analysis of existing methods for determining chemical compatibility reveals the following problems: 1) Determining chemical compatibility through experimental testing carries certain safety risks, and the testing procedures are relatively cumbersome. Limited by the number of experimental personnel and equipment, it is difficult to quickly determine the compatibility of chemicals in a short period of time; 2) Existing testing methods can determine the compatibility of chemical mixtures, but do not provide specific reaction hazards and harmful consequences, including combustion, explosion, gas generation, exothermic reactions, generation of toxic substances, corrosion, etc. Summary of the Invention

[0005] To overcome the problems of existing technologies, this invention provides a method for rapidly determining chemical compatibility based on Raman spectroscopy. This method can quickly determine the hazard of mixing reactions between unknown chemicals, providing technical guidance for avoiding dangers caused by mixing reactions during chemical production, transportation, and storage. It features fast determination speed and high safety.

[0006] To achieve the above objectives, the present invention provides a method for rapidly determining chemical compatibility based on Raman spectroscopy, the method comprising the following steps:

[0007] (1) Use a Raman spectrometer to collect the original spectra of n chemicals whose components and hazards are unknown, and store the Raman shift and intensity signals in the spectrometer;

[0008] (2) The original spectrum of the chemical is preprocessed to obtain the Raman shift and intensity signals of the Raman spectrum of the preprocessed chemical.

[0009] (3) Input the Raman shift and intensity signals of the Raman spectrum of the pretreated chemical into the spectrum feature signal analysis software to determine the characteristic peak positions of the chemical and the corresponding Raman shift values;

[0010] (4) Automatically substitute the Raman shift values ​​corresponding to the characteristic peak positions of the chemical into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software, and obtain the active groups of the chemical through comparison algorithm;

[0011] (5) Automatically input the information of the active group of the chemical into the reaction group analysis software in the Raman spectrometer, and obtain the reaction group information corresponding to the active group of the chemical from the reaction group information database associated with the active group through the comparison algorithm;

[0012] (6) The reaction group information is automatically input into the reactivity analysis software in the Raman spectrometer. The reactivity analysis software contains the chemical reaction group reaction matrix, as well as the hazard information and harmful consequences of the pairwise mixing reaction of the reaction group.

[0013] (7) The reactivity analysis software compares the input chemical reaction group information with the reaction groups in the chemical reaction group reaction matrix through a comparison algorithm. Then, by cross-analyzing the rows and columns of the corresponding reaction groups, the software obtains the corresponding reaction hazard information and harmful consequences at the matrix intersection points.

[0014] (8) The reactivity analysis software provides feedback on the reaction hazards and consequences of chemical mixture reactions using a Raman spectrometer.

[0015] Preferably, in step (1), n ​​is 2 to 30.

[0016] More preferably, in step (1), n ​​is 2 to 20.

[0017] Preferably, in step (2), the preprocessing adopts the preprocessing algorithm integrated in the Raman spectrometer or the preprocessing algorithm in the cloud computing system of the Raman spectrometer.

[0018] Preferably, in step (2), the preprocessing includes data smoothing and baseline correction of the original spectra of the chemical.

[0019] Preferably, in step (3), the spectral feature signal analysis software is the spectral feature signal analysis software integrated into the Raman spectrometer or in a cloud computing system.

[0020] Preferably, in step (3), the method for determining the position of the characteristic peak of the chemical includes: selecting the peak with the largest Raman peak intensity ratio as the characteristic peak by using the Raman spectrum relative intensity calculation formula.

[0021] Preferably, in step (4), the Raman characteristic peak and active group association database contains information on the active groups of the chemical substance and the Raman shift signal values ​​of the characteristic peaks of the corresponding Raman spectra of the chemical substance.

[0022] Preferably, in step (5), the reaction group information database contains information on the active groups of chemical substances and their corresponding reaction group grouping information.

[0023] Preferably, in step (5), the reaction group information database contains 20 to 80 reaction groups.

[0024] Preferably, in step (5), the reaction group includes nitro compounds, organic peroxide compounds, ketone compounds, siloxane compounds, diazonium salt compounds, azo compounds, and amide compounds.

[0025] Preferably, in step (6), the reactivity analysis software is the reactivity analysis software integrated into the Raman spectrometer or in a cloud computing system.

[0026] Preferably, in step (6), the chemical reaction group reaction matrix is ​​formulated based on the statistical analysis of a large number of hazardous accidents caused by chemical mixture reactions and the analysis results of the experimental patterns of chemical mixture reactions.

[0027] The method proposed in this invention can quickly determine the compatibility of a chemical with other chemicals or unknown chemicals simply by collecting Raman spectra of one or more chemicals with unknown components and hazards. It can rapidly obtain the reaction hazards of unknown chemical mixtures and clarify the consequences of chemical mixture reactions, including combustion, explosion, gas generation, exothermic reactions, generation of toxic substances, corrosion, etc. It provides technical guidance for avoiding the dangers caused by mixing reactions during the production, transportation, and storage of chemicals, and is safer. It can conveniently and quickly obtain the hazards and harmful consequences of chemical mixture reactions.

[0028] Compared with the prior art, the present invention has the following technical effects:

[0029] 1) Compared with existing chemical compatibility testing methods, it is safer, and chemical compatibility can be quickly determined in a short time by only collecting the Raman spectrum of the chemical.

[0030] 2) This invention can provide specific information on the hazards and consequences of chemical mixture reactions, and has greater guiding significance for the safe production, storage and transportation of chemicals.

[0031] The method described in this invention can quickly determine the hazard of mixing and reacting unknown chemicals, providing technical guidance for avoiding the dangers caused by mixing and reacting chemicals during production, transportation, and storage. It features fast determination speed and high safety. Attached Figure Description

[0032] Figure 1 This is a flowchart for rapidly determining chemical compatibility based on Raman spectroscopy;

[0033] Figure 2 This is the pre-processed Raman spectrum of blind sample 1# in Example 1;

[0034] Figure 3 This is the pre-processed Raman spectrum of blind sample 2# in Example 1;

[0035] Figure 4 This is the pre-processed Raman spectrum of blind sample 3# in Example 2;

[0036] Figure 5 This is the pre-processed Raman spectrum of blind sample 4# in Example 2;

[0037] Figure 6 This is the pre-treated Raman spectrum of blind sample 5# in Example 3;

[0038] Figure 7 This is the Raman spectrum of blind sample 6# after pretreatment in Example 3. Detailed Implementation

[0039] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0040] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0041] The present invention provides a method for rapidly determining chemical compatibility based on Raman spectroscopy, such as... Figure 1 As shown, it includes the following steps:

[0042] (1) The original spectra of n (≥1) chemicals with unknown components and hazards were collected by Raman spectrometer, and the Raman shift and intensity signals were stored in the spectrometer.

[0043] (2) The original spectrum of the chemical is preprocessed to obtain the Raman shift and intensity signals of the Raman spectrum of the preprocessed chemical.

[0044] (3) Input the Raman shift and intensity signals of the Raman spectrum of the pretreated chemical into the spectrum feature signal analysis software to determine the characteristic peak positions of the chemical and the corresponding Raman shift values;

[0045] (4) Automatically substitute the Raman shift values ​​corresponding to the characteristic peak positions of the chemical into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software, and obtain the active groups of the chemical through comparison algorithm;

[0046] (5) Automatically input the information of the active group of the chemical into the reaction group analysis software in the Raman spectrometer, and obtain the reaction group information corresponding to the active group of the chemical from the reaction group information database associated with the active group through the comparison algorithm;

[0047] (6) The reaction group information is automatically input into the reactivity analysis software in the Raman spectrometer. The reactivity analysis software contains the chemical reaction group reaction matrix, as well as the hazard information and harmful consequences of the pairwise mixing reaction of the reaction group.

[0048] (7) The reactivity analysis software compares the input chemical reaction group information with the reaction groups in the chemical reaction group reaction matrix through a comparison algorithm. Then, by cross-analyzing the rows and columns of the corresponding reaction groups, the software obtains the corresponding reaction hazard information and harmful consequences at the matrix intersection points.

[0049] (8) The reactivity analysis software provides feedback on the reaction hazards and consequences of chemical mixture reactions using a Raman spectrometer.

[0050] The method described in this invention involves collecting Raman spectra of one or more chemicals with unknown components and hazards. By analyzing the characteristic peaks of the Raman spectra, the active groups of the unknown chemicals are identified, and their reaction groups are determined. Simultaneously, through reaction group reaction hazard analysis, the compatibility between unknown chemicals is quickly obtained, i.e., the reaction hazards and harmful consequences after the chemicals are mixed, including combustion, explosion, gas generation, exothermic reaction, generation of toxic substances, corrosion, etc. This method is applicable to the determination of reaction hazards between unknown chemicals.

[0051] In a specific embodiment, n can be 2 to 30 in step (1). In a preferred embodiment, n is 2 to 20 in step (1).

[0052] In the method described in this invention, in step (2), the preprocessing can be performed using the preprocessing algorithm integrated in the Raman spectrometer (i.e., the matching preprocessing algorithm) or the preprocessing algorithm in the cloud computing system of the Raman spectrometer.

[0053] In a specific implementation, in step (2), the preprocessing includes data processing such as data smoothing and baseline correction of the original spectrum of the chemical.

[0054] In the method described in this invention, in step (3), the spectral feature signal analysis software can be the spectral feature signal analysis software integrated into the Raman spectrometer (i.e., the matching software) or in the cloud computing system.

[0055] In a specific implementation, in step (3), the method for determining the position of the characteristic peak of the chemical includes: selecting the peak with the largest Raman peak intensity ratio as the characteristic peak by using the Raman spectrum relative intensity calculation formula.

[0056] In the method described in this invention, in step (4), the Raman characteristic peak and active group association database contains information on the active groups of the chemical substance and the Raman shift signal values ​​of the characteristic peaks of the corresponding Raman spectra of the chemical substance.

[0057] In the method described in this invention, in step (5), the reaction group information database contains information on the active groups of chemical substances and their corresponding reaction group grouping information.

[0058] In a specific embodiment, in step (5), the reaction group information database may contain 20 to 80 reaction groups, for example, 20 reaction groups, 40 reaction groups, 50 reaction groups, 60 reaction groups, 70 or 80 reaction groups. In a preferred embodiment, in step (5), the reaction group information database may contain 20 to 75 reaction groups.

[0059] In the method of the present invention, in step (5), the reaction group may include nitro compounds, organic peroxide compounds, ketone compounds, siloxane compounds, diazonium salt compounds, azo compounds, and amide compounds. In the present invention, the reaction group is not limited to these categories and may also include other categories of compounds.

[0060] In a specific embodiment, in step (6), the reactivity analysis software is the reactivity analysis software integrated (matched) in a Raman spectrometer or in a cloud computing system.

[0061] In the method of the present invention, in step (6), the chemical reaction group reaction matrix is formulated based on the statistical analysis of a large number of hazard accidents of chemical mixture reactions and the analysis results of the rules of chemical mixture reaction tests.

[0062] The Raman spectrometer used in the method of the present invention can be various forms of Raman spectrometers common in the art. In a specific embodiment, for example, it can be a handheld, portable or desktop Raman spectrometer. In a specific embodiment, the method of the present invention realizes the rapid determination of the reaction hazard between unknown chemicals through a chemical compatibility determination program integrated in the spectrometer or a cloud computing system matched with the spectrometer, with strong applicability, convenience and speed.

[0063] The present invention will be described in detail below through examples, but the protection scope of the present invention is not limited thereto.

[0064] Example 1

[0065] Example 1 is used to illustrate the process of quickly determining the compatibility of blind samples 1# and 2# and determining the mixing reaction hazard between the two.

[0066] (1) Blind samples 1# and 2# are respectively filled in 2 mL transparent glass bottles. The original Raman spectra of the two samples are collected respectively using a handheld Raman spectrometer, and the Raman shift and intensity signals corresponding to the original Raman spectra are stored in the handheld Raman spectrometer;

[0067] (2) Using the preprocessing algorithm in the cloud computing system matched with the handheld Raman spectrometer, data processing operations such as data smoothing and baseline correction are performed on the original Raman spectra of blind samples 1# and 2# to obtain the Raman shift and intensity signals of the preprocessed Raman spectra of blind samples 1# and 2#. The preprocessed Raman spectra of blind samples 1# and 2# are shown in Figure 2 and 3 ;

[0068] (3) The Raman shift and intensity signals of the preprocessed blind samples 1# and 2# are automatically input into the spectrum feature signal analysis software in the cloud computing system. The peak with the largest Raman peak intensity ratio of blind samples 1# and 2# is selected as the characteristic peak through the Raman relative intensity calculation formula, thereby determining the characteristic peak position and corresponding Raman shift value of blind samples 1# and 2#.

[0069] (4) The Raman shift values ​​corresponding to the characteristic peaks of blind samples 1# and 2# are automatically substituted into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software. The comparison algorithm in the software obtains that the active group represented by the Raman shift of the characteristic peak of blind sample 1# is (C-NO2) and the active group represented by the Raman shift of the characteristic peak of blind sample 2# is (RRC=O).

[0070] (5) The active group information of blind samples 1# and 2# is automatically input into the reaction group analysis software in the cloud computing system. By comparison algorithm, the reaction group information corresponding to the active group of blind sample 1# is nitroalkane and the reaction group information corresponding to the active group of blind sample 2# is ketone from the 22 reaction group information databases associated with the active group.

[0071] (6) The reaction group information of blind samples 1# and 2# is automatically input into the reactivity analysis software in the cloud computing system. The reactivity analysis software contains a chemical reaction group reaction matrix (22×22), which contains 22 reaction groups, as well as the hazard information and harmful consequences of the two-way mixing reaction of the reaction groups.

[0072] (7) The reactivity analysis software first uses a comparison algorithm to compare the reaction group information of input blind samples 1# and 2# with the reaction groups in the chemical reaction group reaction matrix. Then, it performs cross-analysis by the row where the corresponding nitroalkane reaction group is located and the column where the ketone reaction group is located to obtain the corresponding reaction hazard information and harmful consequences at the matrix intersection point. The result is: the mixture of blind sample 1# and blind sample 2# can trigger a detonation. Therefore, the two are incompatible and should not be mixed.

[0073] (8) The compatibility analysis results of blind samples 1# and 2#, stating that "the mixture of blind sample 1# and blind sample 2# can trigger a detonation, therefore they are incompatible and should not be mixed," were fed back to the user via a handheld Raman spectrometer. In Example 1, the time required from acquiring the spectra of blind samples 1# and 2# from the Raman spectrometer to the cloud computing system returning the compatibility analysis results to the spectrometer was approximately 90 seconds. No mixing reaction experiments were involved in the determination process, ensuring good safety.

[0074] Comparative Example 1

[0075] Referring to "Test Methods for Pyrotechnic Agents Part 17: Compatibility Tests - Differential Thermal Analysis and Differential Scanning Calorimetry GJB5891.17-2006", compatibility tests were conducted on blind samples 1# and 2#.

[0076] (1) Take blind samples 1# and 2# at a mass ratio of 1:1, mix them evenly, and prepare a mixed sample. Weigh 0.7 mg of the mixed sample and pour it into the stainless steel crucible of the differential scanning calorimeter, number it 01, and cover it with a cover plate. At the same time, weigh 0.7 mg of alumina as a reference and pour it into the same crucible, number it 02, and cover it with a cover plate.

[0077] (2) Predict the differential scanning calorimeter for 20 minutes, then place crucibles 01 and 02 into the heating furnace of the differential scanning calorimeter, set the heating rate to 0.5℃ / min, and conduct a heating test on the two crucibles.

[0078] (3) The experiment was stopped when the first decomposition peak appeared on the DSC curve;

[0079] (4) Compare the peak temperature of the mixed sample with the peak temperature of the reference sample, and calculate the change in the first decomposition peak temperature of the mixed sample relative to the reference sample (ΔT). max ), ΔT max If the temperature is greater than 5.0℃, then blind samples 1# and 2# are determined to be incompatible. The test takes approximately 2.5 hours.

[0080] By comparing the compatibility determination process and results of blind samples 1# and 2# in Example 1 and Comparative Example 1, it can be seen that both determinations indicate incompatibility. However, the determination result given in Example 1 is more specific, providing the harmful consequences of mixing blind samples 1# and 2#. Furthermore, Example 1 does not require a mixing reaction experiment, reducing experimental safety risks. In addition, the Raman spectroscopy acquisition and compatibility analysis procedure does not require sample pretreatment, is simple to operate, requires less time, and is computationally efficient, making it more advantageous than the compatibility test in Comparative Example 1.

[0081] Example 2

[0082] Example 2 illustrates the process of rapidly determining the compatibility of blind samples 3# and 4# and identifying the risk of mixed reaction between the two.

[0083] (1) Place blind samples 3# and 4# into 2mL transparent glass bottles respectively, and use a benchtop Raman spectrometer to collect the original Raman spectra of the two samples respectively, and store the Raman shift and intensity signals corresponding to the original Raman spectra in the benchtop Raman spectrometer.

[0084] (2) Using the preprocessing algorithm integrated with the benchtop Raman spectrometer, data processing such as data smoothing and baseline correction were performed on the original Raman spectra of blind samples 3# and 4# to obtain the Raman shift and intensity signals of the preprocessed Raman spectra of blind samples 3# and 4#. The preprocessed Raman spectra of blind samples 3# and 4# are shown below. Figure 4 and 5 ;

[0085] (3) The Raman shift and intensity signals of the pre-processed blind samples 3# and 4# are automatically input into the spectrum feature signal analysis software integrated in the benchtop Raman spectrometer. The peak with the largest Raman peak intensity ratio of blind samples 3# and 4# is selected as the characteristic peak through the Raman relative intensity calculation formula, thereby determining the characteristic peak position and corresponding Raman shift value of blind samples 3# and 4#.

[0086] (4) The Raman shift values ​​corresponding to the characteristic peaks of blind samples 3# and 4# are automatically substituted into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software. The comparison algorithm in the software obtains that the active group represented by the Raman shift of the characteristic peak of blind sample 3# is (Ar-NH2) and the active group represented by the Raman shift of the characteristic peak of blind sample 4# is (-OO-).

[0087] (5) The active group information of blind samples 3# and 4# is automatically input into the reaction group analysis software integrated in the desktop Raman spectrometer. By comparison algorithm, the reaction group information corresponding to the active group of blind sample 3# is obtained from the 73 reaction group information database associated with the active group, which is aromatic amine and the reaction group information corresponding to the active group of blind sample 4# is organic peroxide.

[0088] (6) The reaction group information of blind samples 3# and 4# is automatically input into the reactivity analysis software integrated in the desktop Raman spectrometer. The reactivity analysis software contains a chemical reaction group reaction matrix (73×73), which contains 73 reaction groups, as well as the hazard information and harmful consequences of the pairwise mixing reaction of the reaction groups.

[0089] (7) The reactivity analysis software first uses a comparison algorithm to compare the reaction group information of the input blind samples 3# and 4# with the reaction groups in the chemical reaction group reaction matrix. Then, it performs cross-analysis by the row where the corresponding aromatic amine reaction group is located and the column where the organic peroxide reaction group is located to obtain the corresponding reaction hazard information and harmful consequences at the matrix intersection point. The result is: after the blind samples 3# and 4# are mixed, a slight explosive decomposition may occur after a very short time.

[0090] (8) The compatibility analysis results of blind samples 3# and 4#, “After blind sample 3# and blind sample 4# are mixed, a slight explosive decomposition may occur after a very short time”, are fed back to the user through the tabletop Raman spectrometer.

[0091] In Example 2, the time required from acquiring the spectra of blind samples 3# and 4# using a Raman spectrometer to obtaining the compatibility analysis results was approximately 80 seconds. No mixing reaction experiments were involved in the determination process, indicating good safety.

[0092] Comparative Example 2

[0093] Referring to "Test Methods for Pyrotechnic Agents Part 17: Compatibility Tests - Differential Thermal Analysis and Differential Scanning Calorimetry GJB5891.17-2006", compatibility tests were conducted on blind samples #3 and #4.

[0094] (1) Take blind samples 3# and 4# at a mass ratio of 1:1, mix them evenly, and prepare a mixed sample. Weigh 0.7 mg of the mixed sample and pour it into the stainless steel crucible of the differential scanning calorimeter, number it 01, and cover it with a cover plate. At the same time, weigh 0.7 mg of alumina as a reference and pour it into the same crucible, number it 02, and cover it with a cover plate.

[0095] (2) Predict the differential scanning calorimeter for 20 minutes, then place crucibles 01 and 02 into the heating furnace of the differential scanning calorimeter, set the heating rate to 0.5℃ / min, and conduct a heating test on the two crucibles.

[0096] (3) The experiment was stopped when the first decomposition peak appeared on the DSC curve;

[0097] (4) Compare the peak temperature of the mixed sample with the peak temperature of the reference sample, and calculate the change in the first decomposition peak temperature of the mixed sample relative to the reference sample (ΔT). max ), ΔT max If the temperature exceeds 5.0℃, blind samples #3 and #4 are determined to be incompatible. The test takes approximately 3 hours.

[0098] By comparing the compatibility determination process and results of blind samples 3# and 4# in Example 2 and Comparative Example 2, it can be seen that both determinations indicate incompatibility. However, the determination result given in Example 2 is more specific, providing the harmful consequences of mixing blind samples 3# and 4#. Furthermore, Example 2 does not require a mixing reaction experiment, reducing experimental safety risks. In addition, the Raman spectroscopy acquisition and compatibility analysis procedure does not require sample pretreatment, is simple to operate, requires less time, and is computationally efficient, making it more advantageous than the compatibility test in Comparative Example 2.

[0099] Example 3

[0100] Example 3 illustrates the process of rapidly determining the compatibility of blind samples 5# and 6# and identifying the risk of mixed reactions between the two.

[0101] (1) Place blind samples 5# and 6# into 2mL transparent glass bottles respectively, and use a benchtop Raman spectrometer to collect the original Raman spectra of the two samples respectively, and store the Raman shift and intensity signals corresponding to the original Raman spectra in the benchtop Raman spectrometer.

[0102] (2) Using the preprocessing algorithm integrated with the benchtop Raman spectrometer, data processing such as data smoothing and baseline correction were performed on the original Raman spectra of blind samples 5# and 6# to obtain the Raman shift and intensity signals of the preprocessed Raman spectra of blind samples 5# and 6#. The preprocessed Raman spectra of blind samples 5# and 6# are shown below. Figure 6 and 7 ;

[0103] (3) The Raman shift and intensity signals of the pre-processed blind samples 5# and 6# are automatically input into the spectrum feature signal analysis software integrated in the desktop Raman spectrometer. The peak with the largest Raman peak intensity ratio of blind samples 5# and 6# is selected as the characteristic peak through the Raman relative intensity calculation formula, thereby determining the characteristic peak position and corresponding Raman shift value of blind samples 5# and 6#.

[0104] (4) The Raman shift values ​​corresponding to the characteristic peaks of blind samples 5# and 6# are automatically substituted into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software. The comparison algorithm in the software obtains that the active group represented by the Raman shift of the characteristic peak of blind sample 5# is (Ar-OH) and the active group represented by the Raman shift of the characteristic peak of blind sample 6# is -NO2.

[0105] (5) The active group information of blind samples 5# and 6# is automatically input into the reaction group analysis software integrated in the desktop Raman spectrometer. By comparison algorithm, the reaction group information corresponding to the active group of blind sample 5# is obtained from the 68 reaction group information database associated with the active group, which is phenolic and the reaction group information corresponding to the active group of blind sample 6# is nitro.

[0106] (6) The reaction group information of blind samples 5# and 6# is automatically input into the reactivity analysis software integrated in the desktop Raman spectrometer. The reactivity analysis software contains a chemical reaction group reaction matrix (68×68), which contains 68 reaction groups, as well as the hazard information and harmful consequences of the pairwise mixing reaction of the reaction groups.

[0107] (7) The reactivity analysis software first uses a comparison algorithm to compare the reaction group information of the input blind samples 5# and 6# with the reaction groups in the chemical reaction group reaction matrix. Then, it performs cross-analysis by the row where the corresponding phenolic reaction group is located and the column where the corresponding nitro reaction group is located to obtain the corresponding reaction hazard information and harmful consequences at the matrix intersection point: After blind sample 5# and blind sample 6# are mixed, a rapid combustion reaction may occur.

[0108] (8) The compatibility analysis results of blind samples 5# and 6#, “After mixing blind sample 5# and blind sample 6#, a rapid combustion reaction may occur,” are fed back to the user through a desktop Raman spectrometer.

[0109] In Example 3, the time required from acquiring the spectra of blind samples 5# and 6# using a Raman spectrometer to obtaining the compatibility analysis results was approximately 85 seconds. No mixing reaction experiments were involved in the determination process, indicating good safety.

[0110] Comparative Example 3

[0111] Referring to "Test Methods for Pyrotechnic Agents Part 17: Compatibility Tests - Differential Thermal Analysis and Differential Scanning Calorimetry GJB5891.17-2006", compatibility tests were conducted on blind samples #5 and #6.

[0112] (1) Take blind samples 5# and 6# at a mass ratio of 1:1, mix them evenly, and prepare a mixed sample. Weigh 0.7 mg of the mixed sample and pour it into the stainless steel crucible of the differential scanning calorimeter, number it 01, and cover it with a cover plate. At the same time, weigh 0.7 mg of alumina as a reference and pour it into the same crucible, number it 02, and cover it with a cover plate.

[0113] (2) Predict the differential scanning calorimeter for 20 minutes, then place crucibles 01 and 02 into the heating furnace of the differential scanning calorimeter, set the heating rate to 0.5℃ / min, and conduct a heating test on the two crucibles.

[0114] (3) The experiment was stopped when the first decomposition peak appeared on the DSC curve;

[0115] (4) Compare the peak temperature of the mixed sample with the peak temperature of the reference sample, and calculate the change in the first decomposition peak temperature of the mixed sample relative to the reference sample (ΔT). max ), ΔT max If the temperature is greater than 5.0℃, then blind samples #5 and #6 are determined to be incompatible. The test takes approximately 2.6 hours.

[0116] By comparing the compatibility determination process and results of blind samples 5# and 6# in Example 3 and Comparative Example 3, it can be seen that both determinations indicate incompatibility. However, the determination result given in Example 3 is more specific, providing the harmful consequences of mixing blind samples 5# and 6#. Furthermore, Example 3 does not require a mixing reaction experiment, reducing experimental safety risks. In addition, the Raman spectroscopy acquisition and compatibility analysis procedure does not require sample pretreatment, is simple to operate, requires less time, and is computationally efficient, making it more advantageous than the compatibility test in Comparative Example 3.

[0117] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A method for rapidly determining chemical compatibility based on Raman spectroscopy, characterized in that, The method includes the following steps: (1) Use a Raman spectrometer to collect the original spectra of n chemicals whose components and hazards are unknown, and store the Raman shift and intensity signals in the spectrometer; (2) The original spectrum of the chemical is preprocessed to obtain the Raman shift and intensity signals of the Raman spectrum of the preprocessed chemical. (3) Input the Raman shift and intensity signals of the Raman spectrum of the pretreated chemical into the spectrum feature signal analysis software to determine the characteristic peak position of the chemical and the corresponding Raman shift value; (4) Automatically substitute the Raman shift values ​​corresponding to the characteristic peak positions of the chemical into the Raman characteristic peak and active group association database in the spectrum characteristic signal analysis software, and obtain the active groups of the chemical through the comparison algorithm; (5) Automatically input the active group information of the chemical into the reaction group analysis software in the Raman spectrometer, and obtain the reaction group information corresponding to the active group of the chemical from the reaction group information database associated with the active group through the comparison algorithm. The reaction group information database contains the active group information of the chemical substance and its corresponding reaction group grouping information. (6) The reaction group information is automatically input into the reactivity analysis software in the Raman spectrometer. The reactivity analysis software contains the chemical reaction group reaction matrix, as well as the hazard information and harmful consequences of the pairwise mixing reaction of the reaction group. (7) The reactivity analysis software compares the input chemical reaction group information with the reaction group in the chemical reaction group matrix through a comparison algorithm. Then, by cross-analyzing the rows and columns of the corresponding reaction groups, the software obtains the corresponding reaction hazard information and harmful consequences at the matrix intersection points. (8) The reactivity analysis software provides feedback on the reaction hazard information and harmful consequences of chemical mixture reactions through a Raman spectrometer.

2. The method according to claim 1, characterized in that, In step (1), n ​​is 2 to 30.

3. The method according to claim 2, characterized in that, In step (1), n ​​is 2 to 20.

4. The method according to claim 1, characterized in that, In step (2), the preprocessing adopts the preprocessing algorithm integrated in the Raman spectrometer or the preprocessing algorithm in the cloud computing system of the Raman spectrometer.

5. The method according to claim 1, characterized in that, In step (2), the preprocessing includes data smoothing and baseline correction of the original spectra of the chemicals.

6. The method according to claim 1, characterized in that, In step (3), the spectral feature signal analysis software is either integrated into the Raman spectrometer or is a spectral feature signal analysis software in a cloud computing system.

7. The method according to claim 1, characterized in that, In step (3), the method for determining the position of the characteristic peak of the chemical includes: selecting the peak with the largest Raman peak intensity ratio as the characteristic peak by using the Raman spectrum relative intensity calculation formula.

8. The method according to claim 1, characterized in that, In step (4), the Raman characteristic peak and active group association database contains information on the active groups of chemical substances and the Raman shift signal values ​​of the characteristic peaks of the corresponding Raman spectra of chemical substances.

9. The method according to claim 1, characterized in that, In step (5), the reaction group information database contains 20 to 80 reaction groups.

10. The method according to claim 1, characterized in that, In step (5), the reaction group includes nitro compounds, organic peroxide compounds, ketone compounds, siloxane compounds, diazonium salt compounds, azo compounds and amide compounds.

11. The method according to claim 1, characterized in that, In step (6), the reactivity analysis software is the reactivity analysis software integrated into the Raman spectrometer or in a cloud computing system.

12. The method according to claim 1, characterized in that, In step (6), the chemical reaction group reaction matrix is ​​formulated based on the statistical analysis of a large number of hazardous accidents caused by chemical mixture reactions and the analysis results of the experimental patterns of chemical mixture reactions.

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